CN202808347U - Device for preparing active calcium hydride - Google Patents
Device for preparing active calcium hydride Download PDFInfo
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- CN202808347U CN202808347U CN 201220452495 CN201220452495U CN202808347U CN 202808347 U CN202808347 U CN 202808347U CN 201220452495 CN201220452495 CN 201220452495 CN 201220452495 U CN201220452495 U CN 201220452495U CN 202808347 U CN202808347 U CN 202808347U
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- hydrogen
- hydrolith
- calcium hydride
- active calcium
- tube
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Abstract
本实用新型涉及活性氢化钙的制备技术，旨在提供一种制备活性氢化钙的装置。该装置包括电加热炉，该电加热炉具有水平横置的炉管，炉管外裹保温层，其内部套设一根石英反应管；石英反应管的一端内置石棉栅格，在石棉栅格中间插入通氢气的管路，另一端直接敞开接通大气。通过利用本实用新型所进行的活性氢化钙制备方法，其制备工艺简洁，操作条件平和，环境污染轻，资源消耗少；制得的活性氢化钙固体粉末，能在水中同时释放出氢气和氧气，既可用作清洁能源的储存载体，同时释放出的氢负离子具有人体保健作用。
The utility model relates to the preparation technology of active calcium hydride and aims to provide a device for preparing active calcium hydride. The device includes an electric heating furnace. The electric heating furnace has a furnace tube horizontally placed. The furnace tube is wrapped with an insulating layer and a quartz reaction tube is set inside; an asbestos grid is built in one end of the quartz reaction tube. A hydrogen pipeline is inserted in the middle, and the other end is directly opened to the atmosphere. By using the method for preparing active calcium hydride of the present invention, the preparation process is simple, the operating conditions are gentle, the environmental pollution is light, and the resource consumption is low; the prepared active calcium hydride solid powder can simultaneously release hydrogen and oxygen in water, It can be used as a storage carrier for clean energy, and the hydrogen negative ions released at the same time have the effect of human health care.
Description
Technical field
The utility model relates to the active hydrolith (CaH of a kind of particular chemicals
2Preparation facilities 2H2O) especially is applicable to come single stage method to synthesize the process of particular chemicals by the control chemical reaction condition, belongs to a kind of technology of gas and solid phase catalyzing preparation.
Background technology
Hydrogen and oxygen as energy carrier have that the source is abundant, energy density is high, environmental protection, storing mode and utilize the characteristics such as various informative.In the new forms of energy system, Hydrogen Energy will become lays equal stress on electric energy and complementary terminal secondary energy, permeates and serve all respects of social and economic activities, occupies critical role in the energy security of country and environment protection.At present, many countries such as the U.S., European Union, Canada, Japan, China, Korea S and Brazil and area are all in the develop actively Hydrogen Technology.In the technical system that Hydrogen Energy is utilized, hydrogen storage and transmission ﹠ distribution technology have become the research focus of countries in the world as the key link in the practical application.Particularly, be to realize that Hydrogen Energy uses in the mass-producing in the fields such as public transport and mobile communication, hydrogen storage and transmission ﹠ distribution technology must possess safety, make things convenient for and the essential characteristic such as efficient.Therefore, the hydrogen storage ability is still current main research emphasis and technical bottleneck.Existing storing mode mainly contains high-pressure gaseous storage hydrogen, low temperature liquid storage hydrogen and solid-state absorption or in conjunction with three major types such as Chu Qing, wherein front two classes also do not have the technical superioritys such as safe, reliable and convenient, and the 3rd class mainly be by Chemical bond or physical adsorption method with storing hydrogen in solid-state material, possess process convenient, energy density is high and the advantage such as safe and reliable, be considered to current tool and realize property and the most promising a kind of storage hydrogen mode, if can adsorb simultaneously the then more worth exploration of mode of store up oxygen.
Existing large quantity research and report relate to the exploitation of novel hydrogen storage material and mode both at home and abroad, can discharge a large amount of high-purity hydrogens when wherein the material of hydrolith and so on is owing to the chance water decomposition, can be used as light hydrogen propellant, can provide high efficient energy sources when being applied to field work, and the hydride ion that discharges has body-care effect etc., is just becoming one of present exploitation focus because it is of many uses.As in up-to-date open and representative patented technology, CN102198933A discloses the preparation method of a kind of novel high-capacity composite hydrogen storage material calcium borohydride/ammino lithium borohydride; The CN100595129C utility model a kind of nano calcium hydride and preparation method, wherein relate to nano-scale metal hydride and preparation method; CN102100699A discloses a kind of coral calcium hydroxide and arginic composition and application thereof, it can discharge negative hydrogen ion after meeting water decomposition, can be applicable to prepare the healthcare products that improve body immunity, or for the preparation of medicine or the healthcare products for the treatment of cardiovascular and cerebrovascular diseases; CN102146027A then with hydrolith as one of catalyzer, a kind of preparation technology of muskone etc. is disclosed.
Resolve hydrolith (CaH according to known " chemical dictionary "
2) usually at high temperature pass into purifying hydrogen of hydrogen reaction by about 99.5% redistilled calcium of purity and make.It does not all react with dry air, nitrogen, chlorine at normal temperatures, but at high temperature can with above-mentioned gas generation chemical reaction, generate respectively calcium oxide, carbide of calcium, calcium chloride.Therefore, more than and the defectives such as other conventional physical chemistry preparation methods exist that the final reacting product composition is difficultly held, the difficult control of reaction conditions, preparation cost is higher and preparation efficiency is lower, particularly so far there are no can be with the hydrolith report of chemisorption storage hydrogen and storage oxygen simultaneously.
The utility model content
The technical problems to be solved in the utility model is, overcomes deficiency of the prior art, and a kind of device for preparing active hydrolith is provided.
Be the technical solution problem, solution of the present utility model is:
The utility model provides a kind of horizontal tube electrical heater for aforementioned active hydrolith preparation method, comprises electrical heater, and this electrical heater has the horizontal boiler tube of level, and boiler tube is wrapped up in thermal insulation layer outward, its inner sheathed crystal reaction tube; The built-in asbestos grid of one end of crystal reaction tube inserts the pipeline that leads to hydrogen in the middle of the asbestos grid, the other end directly opens wide connects atmosphere.
As a kind of improvement, described electrical heater is connected to microcomputer controller and realizes heating control by it by wire; The rated output of electrical heater is 2 kilowatts, and maximum heating temperature is 1000 ℃; The internal diameter of described boiler tube is 6 centimetres, and length is 90 centimetres; The external diameter of described crystal reaction tube is 5 centimetres, and length is 120 centimetres, and wall thickness is 0.2 centimetre; The asbestos grid diameter of described quartz reaction tube end is 4.8 centimetres, and thickness is 0.5 centimetre, and the aperture at its intubate place, center is 0.6 centimetre.Built-in crystal reaction tube can hold material quantity 120～200 and restrain/criticize.
Intermittent type, one-step synthesis process are adopted in the preparation of active hydrolith, specifically comprise the steps:
(1) raw material hydrogenation calcium powder evenly is interspersed in the crystal reaction tube stage casing of horizontal tube electrical heater;
(2) the equal blow-by in the two ends of crystal reaction tube, and be in the air ambient of constant pressure and dry; Continue to pass into dry hydrogen with tiny flow quantity, it is 0.1～0.2 l/h that the flow of control hydrogen makes the hydrogen usage that transforms every gram hydrolith; The control furnace temperature is 300 ℃～700 ℃, and the reaction times is 8～12 hours; Under this reaction conditions, hydrolith makes active hydrolith pressed powder owing to adsorbing simultaneously hydrogen and oxygen, and its molecular formula is CaH
22H2O.
The chemical equation of reaction process is as follows:
CaH
2(S) + H
2(g) + O
2(g)→CaH
2·2H·2O (S) （1）
According to theory of ionization in chemisorption principle, the aqueous solution etc., the molecular formula of active hydrolith can be described as CaH
2.2H.2O, its sign be, under the control special reaction condition, combine simultaneously hydrogen and oxygen in the chemisorption mode in the hydrolith molecular structure, its molecular weight is 76.09.Physical aspect is canescence class powder.Its chemical property shows as, and is stable in drying medium, having no hydrogen and oxygen desorption below 1000 ℃, and the test result spectrogram that sees for details among the appended embodiment of this specification sheets is illustrated.Fast decoupled ionization in liquid water, with discharging hydrogen and oxygen, its reaction formula is described below:
CaH
2·2H·2O (S)+4H
2O(L)→[Ca
2++2OH
-+ H
3O
++ H
3O
-](aq)+2H
2(g)↑+2O
2(g)↑（2）
In the formula, H
3O
+And H
3O
-Represent respectively by the positive and negative hydrogen ion hydrate of aquation, i.e. H
+And H
-Rear mark (S), (L), (aq) and (g) represent respectively the material phases such as solid, liquid, the aqueous solution be gentle wherein.
In the utility model, reaction must be to carry out in logical spacious silica tube environment, because hydrogen dangerous property at high temperature, so to accurately be controlled to tiny flow quantity, and oxygen does not need to control its concrete intake from atmospheric environment.One of the utility model core point is exactly accurately to control reaction conditions (can be realized by the controller of micro computer programming).Comprehensively shown by multiple detected results such as electro-chemical test, EDS power spectrum and He-TDP desorptions, at last in the synthetic active hydrolith simultaneously chemisorption hydrogen and oxygen.
Compared with prior art, advantage of the present utility model is:
By utilizing active hydrolith preparation method of the present utility model, its preparation technology is succinct, operational condition is gentle, environmental pollution is light, and resource consumption is few, and prepared active hydrolith is in its chemical reaction process, owing to hydrolith adsorbs hydrogen and oxygen makes active hydrolith pressed powder simultaneously, can discharge simultaneously hydrogen and oxygen in water, both can be used as the storage carrier of clean energy, the hydride ion that discharges simultaneously has the body-care effect.
Description of drawings
Fig. 1 is active hydrolith preparation facilities of the present utility model.
Fig. 2 is the electrolyzer that the negative hydrogen ion concentration determination shares in water electrolysis hydrogen production and the active hydrolith hydrolyzed solution.
Fig. 3 is EDS power spectrum element determination result.
Fig. 4 is that the XRD phase is measured collection of illustrative plates.
Fig. 5 is the TCD signal collection of illustrative plates of He-TDP desorption.
Fig. 6 is the MS signal collection of illustrative plates of He-TDP desorption.
Reference numeral among the figure: 1, hydrogen inlet pipe, 2, the horizontal tube electrical heater, 3, the asbestos grid, 4, the powder material of reaction, 5, crystal reaction tube, 6, direct supply, 7, electrolyzer, 8, electrode.
Embodiment
Active hydrolith (CaH in the utility model
22H2O) preparation method adopts intermittent type, one-step synthesis process.Mainly be under the special reaction condition of controlling, so that hydrolith while chemisorption hydrogen and oxygen, the active hydrolith that finally makes can discharge hydrogen and oxygen simultaneously in water, both can be used as the storage carrier of clean energy, and meet the hydride ion that water decomposition discharges and have the body-care effect, have the physiological property of coral calcium hydroxide goods concurrently.This is up to now to have no in the known utility model patent technology.Obtained a kind ofly can make things convenient for, safety and store up reliably hydrogen and oxygen, again can be when needed, the type material of rapid, high volume ground release hydrogen and oxygen simultaneously.
Below in conjunction with drawings and Examples the utility model is further specified.
One of embodiment 1 active hydrolith preparation experiment.
For the experiment preparation facilities shown in Fig. 1, its key points for operation are:
Raw material hydrogenation calcium powder (commercial) is distributed in crystal reaction tube 5 stage casings and completion system assembling in right amount;
In the atmospheric air environment, connect electrolyzer 7(shown in Figure 2 first for the preparation of, be used for test afterwards), the dry hydrogen that passes into its brine electrolysis generation flow to stable;
1. start horizontal tube electrothermal oven 2 in limited time and be rapidly heated, micro computer is regulated control hot(test)-spot temperature value, timing register control reaction times, slow cooling;
2. discharging after the cooling, heat preservation and dryness, metering.
Its reaction conditions is controlled to be:
Major control hot(test)-spot temperature and hydrogen flowing quantity are carried out in the experiment preparation in the constant pressure and dry air ambient.
The control hot(test)-spot temperature amounts to 12 hours reaction times at 700 ℃.Hydrogen flowing quantity is controlled to be 0.2 l/h of the hydrogen flowing quantity that transforms every gram hydrolith.
Experimental result: active hydrolith actual recovery is 98%.
Two of embodiment 2. active hydrolith preparation experiments.
Experimental installation is identical with embodiment 1 with key points for operation.The control hot(test)-spot temperature amounts to 10 hours reaction times at 300 ℃, and hydrogen flowing quantity is controlled to be 0.1 l/h of the hydrogen flowing quantity that transforms every gram hydrolith.
Experimental result: active hydrolith actual recovery is 92%.
Negative hydrogen ion concentration determination in the embodiment 3. active hydrolith hydrolyzed solutions.
Measuring method: direct current solution.
For the experiment test device shown in Fig. 2, its equipment consists of:
1. dc current regulator power supply (commercial).
2. electrolyzer 7: self-control is comprised of electrode 8 assemblies, cell body and other related accessory.Cell body is a rectangular box type container.
3. electrode 8 assemblies are the electrolyzer internals that combined the series connection of three Room by 4 graphite electrode plates with multipole type.
Its key points for operation are:
1. adopt constant voltage control, it is 6.0 volts that total voltage is set, and each tank room real work voltage is about 2 volts.
2. get active hydrolith style 120 grams that embodiment 1 makes, through 1.5 liters of the clean hydrolyzed solutions that obtain after fully being hydrolyzed, clarifying, filtering, disposable input electrolyzer 7 is initial liquid to be determined.
3. start direct supply 6 at normal pressure, normal temperature, open timing electrolysis under the static conditions.
4. record measured data, the voltage when mainly comprising steady state, electric current and conduction time etc.
5. determine the electrolysis terminal point: along with the electrolysis process, the negative hydrogen ion density loss, electric current descends, and when confirming that most of negative hydrogen ion has discharged, is the electrolysis terminal point.
6. test-results is carried out data processing, try to achieve negative hydrogen ion concentration [H in this activity hydrolith hydrolyzed solution
-] approach.
Determination data gathers:
The experimental data that table 1 electrochemical process is measured negative hydrogen ion concentration in the active hydrolith hydrolyzed solution gathers
The data processing method of test result:
As follows according to the electrode reaction equation that known electrochemical thermodynamics principle is write out in this electrolytic trial:
Anode
Negative electrode
Total reaction
According to Faraday's law: 1 faraday's electric weight is 96500 coulombs, namely 26.8 ampere-hours.Accumulative total is passed through electric weight 4.74 ampere-hours, 1.5 liters of hydrolyzed solutions, then negative hydrogen ion concentration in this test as known from Table 1:
Conclusion: negative hydrogen ion concentration approach is 0.17 mol/L in the active hydrolith hydrolyzed solution that this test records.
The EDS power spectrum element determination result of embodiment 4. active hydroliths.
In Fig. 3, provided the chief component of the EDS power spectrum element determination of active hydrolith pressed powder.
The XRD phase of embodiment 5. active hydroliths is measured collection of illustrative plates.
In Fig. 4, the XRD phase that has provided active hydrolith pressed powder is measured the collection of illustrative plates result.
The He-TDP desorption collection of illustrative plates of embodiment 6. active hydroliths.
In Fig. 5,6, provided the He-TDP desorption collection of illustrative plates result of active hydrolith pressed powder.Its condition determination is:
1. test event hydrogen adsorptive capacity.
2. testing tool Micromeritics Autochem 2910.
3. example weight 0.1 restrains.
4. reactor is U-shaped silica tube.
5. test is He with gas, flow 10 ml/min.
6. sample is pressed powder.
7. test procedure: helium purge is 30 minutes under the room temperature, helium 99.999%, and 10 ℃/minute of program control temperature rise rates in helium atmosphere then, TCD and MS detect tail gas atmosphere.
The utility model makes the main application of active hydrolith:
1, is used as the storage carrier of clean energy
Active hydrolith CaH
22H2O is the pressed powder of the double storage of Chu Qing oxygen, can discharge fast H when meeting water decomposition
2: O
2The geseous fuel of=2:1, the ejecta smoke dust, toxicological harmless is without CO
2, the negative hydrogen ion in the aqueous solution has positive elimination effect to the ozone pollution in the atmosphere.
2, as the body-care effect
Contain the biological products of active hydrolith with an amount of soup 0.1 gram-0.3 gram of swallowing, can in human body, be hydrolyzed.The negative hydrogen ion that discharges can be resisted free radical, strengthens body immunity.Excess is hydrogen, oxygen, water and calcium, all has no side effect.Also can be directly used in the healthcare products that a kind of pure inorganic molecule of preparation consists of.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220452495 CN202808347U (en) | 2012-09-06 | 2012-09-06 | Device for preparing active calcium hydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220452495 CN202808347U (en) | 2012-09-06 | 2012-09-06 | Device for preparing active calcium hydride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202808347U true CN202808347U (en) | 2013-03-20 |
Family
ID=47867268
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201220452495 Expired - Lifetime CN202808347U (en) | 2012-09-06 | 2012-09-06 | Device for preparing active calcium hydride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN202808347U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826511A (en) * | 2012-09-06 | 2012-12-19 | 浙江华康药业股份有限公司 | Method and device for preparing active calcium hydride |
| CN106629603A (en) * | 2016-12-28 | 2017-05-10 | 北京有色金属研究总院 | Preparation method of low-nitrogen and high-purity calcium hydride |
-
2012
- 2012-09-06 CN CN 201220452495 patent/CN202808347U/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826511A (en) * | 2012-09-06 | 2012-12-19 | 浙江华康药业股份有限公司 | Method and device for preparing active calcium hydride |
| CN102826511B (en) * | 2012-09-06 | 2014-04-30 | 浙江华康药业股份有限公司 | Method and device for preparing active calcium hydride |
| CN106629603A (en) * | 2016-12-28 | 2017-05-10 | 北京有色金属研究总院 | Preparation method of low-nitrogen and high-purity calcium hydride |
| CN106629603B (en) * | 2016-12-28 | 2019-03-22 | 北京有色金属研究总院 | A kind of preparation method of the high-purity calcium hydride of low nitrogen |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20130320 Effective date of abandoning: 20140430 |
|
| RGAV | Abandon patent right to avoid regrant |