JP4813640B2 - Method for producing cellulose ether - Google Patents
Method for producing cellulose ether Download PDFInfo
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- JP4813640B2 JP4813640B2 JP2000177875A JP2000177875A JP4813640B2 JP 4813640 B2 JP4813640 B2 JP 4813640B2 JP 2000177875 A JP2000177875 A JP 2000177875A JP 2000177875 A JP2000177875 A JP 2000177875A JP 4813640 B2 JP4813640 B2 JP 4813640B2
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- pulp
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- cellulose ether
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Description
【0001】
【発明の属する技術分野】
本発明は、セルロースエーテルの原料およびその他の工業用途に利用される、粉末状パルプの製造方法に関するものである。
【0002】
【従来の技術】
粉末状のパルプはセルロースエーテルの原料、その他工業用に用いられる。
シート状パルプを粉砕して粉末状パルプを得ようとするとき、従来は、シート状パルプの単位面積当たりの重量に着目したものはなかった。
【0003】
【本発明が解決しようとする課題】
従来の技術は、シート状パルプを粉砕する際、粉砕機の粉砕動力原単位が非常に大きく、また、パルプの主成分であるセルロースの重合度の低下が著しいため、得られた粉末状パルプを原料にして製造したセルロースエーテルの水溶液粘度が低いことが課題だった。
本発明は、シート状パルプを粉砕して粉末状パルプを得ようとする時の、粉砕動力原単位を低減し、また、セルロースの重合度の低下を軽減することを目的とする。
【0004】
【課題を解決するための手段】
本発明は、上記課題の解決のため、シート状パルプを粉砕して粉末状パルプを得ようとするとき、粉砕原料であるシート状パルプの面積当たりの重量をコントロールする。コットンリンターパルプは面積当たりの重量が700〜1200g/m 2 のシート状パルプ、ウッドパルプは900〜1200g/m 2 のシート状パルプを用いる。
【0005】
【発明の実施の形態】
以下、本発明を詳細に説明する。
本発明のコットンリンターパルプとは、綿の種子に生ずる繊維を原料にして得られるパルプである。また、本発明のウッドパルプとは、木材を原料にして得られるパルプである。コットンリンターパルプおよびウッドパルプに含まれるセルロースの重合度は限定しないが、通常、粘度測定法による重量平均重合度(以下、「Dpw」と略す。)が、500〜8,000のものを用いる。
【0006】
パルプは、その形状に基づき、シート状パルプ、粉末状パルプ、綿状パルプに分類される。本発明の対象となるシート状パルプは、好ましくは厚さ3mm以下の平板状パルプである。
シート状パルプの製造方法は、特に限定されない。
【0007】
シート状パルプは、通常、数重量%〜10重量%程度の水分を含んでいる。本発明で言う、「面積当たりの重量」とは、水分の重量を含めない重量である。水分含量により、面積当たりの重量は見掛け上変動するが、水分が10重量%以下であれば本発明の効果に影響を与えない。すなわち、水分以外の重量に着目することが必要である。
水分の重量を含めない面積当たりの重量の求め方は、以下の式による。
W = M×(1― 0.01x)/S
ここで、Wは水分の重量を含めない面積当たりの重量、Mは面積Sのシート状パルプの水分込みの重量、xはこのパルプの水分(重量%)である。パルプの水分の測定は、パルプ片2gを105℃で1時間以上乾燥した時の減量%である。
【0008】
本発明で言うシート状パルプの面積は、一片のシート状パルプを六面体としてとらえた場合、六面のうち最も面積の大きい面の面積をさす。
本発明で用いるコットンリンターパルプは、面積当たりの重量が650g/m2以上、好ましくは700〜1,200g/m2のシート状パルプ、ウッドパルプは、900g/m2以上、好ましくは900〜1,200g/m2のシート状パルプを用いる。それより小さいものは、本発明の効果である、動力原単位の低減効果と重合度低下の軽減効果が得られない場合がある。
なお、動力原単位とは、一定重量のシート状パルプを粉砕して一定の平均粒径の粉末状パルプを得るためのパルプ粉砕機の所要電力をいう。
【0009】
本発明で用いるシート状パルプの厚みおよび見掛け密度は特に限定しないが、通常、厚みは0.5〜2.5mm、見掛け密度は0.4〜1.0g/mlのものを用いる。面積当たりの重量はシートの厚みと見掛け密度の積で表わせるため、厚みが一定であれば、見掛け密度のより大きなものを、見掛け密度が一定なら厚みのより大きなものを用いるのが好ましい。むろん、面積当たりの重量が、コットンリンターパルプでは650g/m2以上、ウッドパルプでは900g/m2以上を満たすものでなければならない。
【0010】
本発明で用いるシート状パルプは、粉砕前に、粉砕機の構造に応じて、粉砕機に投入しやすい適当な大きさおよび形状、例えば0.5〜2cm角のチップ状にすることができる。
本発明の粉砕に用いる粉砕機は、ナイフミル、衝撃粉砕機、竪型ローラーミル等が挙げられるが、特に限定されない。
本発明で得られる粉末状パルプの平均粒径は1,000μm以下、好ましくは60〜500μmである。平均粒径が1,000μmを超えると、粉末状パルプの流動性が低下し、粉体としての取り扱いが困難になるおそれがある。
【0011】
本発明のセルロースエーテルは、公知の方法、たとえば粉末状パルプに水酸化ナトリウム、水酸化カリウム等のアルカリを加えてアルカリセルロースとした後に、塩化メチル、酸化プロピレン、酸化エチレン等のエーテル化剤を加えて加熱することにより得られる。
【0012】
【実施例】
以下、本発明を実施例及び比較例によってさらに詳細に説明するが、本発明はこれら実施例の記載に限定されるものではない。
実施例1
面積当たりの重量が750g/m2、カドキセン溶液粘度測定法によるDpwが7,000のシート状のコットンリンターパルプをナイフミル(HA―2542:株式会社朋来鉄工所製)で粉砕した。粉砕動力原単位は0.17kwh/kgだった。得られた粉末状パルプの平均粒径は250μmであり、Dpwは4,770であった。
粉砕したパルプ100重量部を内部撹拌機つきの反応器に入れ、十分に窒素置換した後、水酸化ナトリウム123重量部、メトキシル基置換のために塩化メチル80重量部、ヒドロキシプロポキシル基置換のために酸化プロピレン21重量部を加え、40〜100℃で反応させ、熱水でヒドロキシプロピルメチルセルロースに対し残塩分が1重量%程度になるまで精製し、その後乾燥して含有水分が1.2重量%の原料ヒドロキシプロピルメチルセルロースを得た。この原料ヒドロキシプロピルメチルセルロースは、メトキシル置換度が1.4、ヒドロキシプロポキシル基置換度が0.2であった。なお、置換度は1グルコースユニット当たりに導入された置換基数を示す。得られたヒドロキシプロピルメチルセルロースの1重量%水溶液の粘度は、19,000mPa・sだった。
【0013】
実施例3
面積当たりの重量が1200g/m2であるシート状のコットンリンターパルプを用いる以外は実施例1と同様の操作を行った。粉砕動力原単位は0.10kwh/kg、得られた粉末状パルプの平均粒径は250μmであり、Dpwは4,850であった。ヒドロキシプロピルメチルセルロースの1重量%水溶液の粘度は、19,500mPa・sだった。
【0014】
実施例3
面積当たりの重量が950g/m2、Dpwが4,000のシート状のウッドパルプを用いる以外は実施例1と同様の操作を行った。粉砕動力原単位は0.13kwh/kg、得られた粉末状パルプの平均粒径は120μmであり、Dpwは3,060であった。ヒドロキシプロピルメチルセルロースの1重量%水溶液の粘度は、8,000mPa・sだった。
【0015】
実施例4
面積当たりの重量が1,200g/m2、Dpwが4,000のシート状のウッドパルプを用いる以外は実施例1と同様の操作を行った。粉砕動力原単位は0.10kwh/kg、得られた粉末状パルプの平均粒径は120μmであり、Dpwは3,150であった。ヒドロキシプロピルメチルセルロースの1重量%水溶液の粘度は、8,200mPa・sだった。
【0016】
比較例1
面積当たりの重量が570g/m2のシート状のコットンリンターパルプを用いる以外は実施例1と同様の操作を行った。粉砕動力原単位は0.25kwh/kg、得られた粉末状パルプの平均粒径は250μm、Dpwは4,500であり、ヒドロキシプロピルメチルセルロースの1重量%水溶液の粘度は、15,000mPa・sだった。
【0017】
比較例2
面積当たりの重量が750g/m2のシート状のウッドパルプを用いる以外は実施例1と同様の操作を行った。粉砕動力原単位は0.17kwh/kg、得られた粉末状パルプの平均粒径は120μm、Dpwは2,390であり、ヒドロキシプロピルメチルセルロースの1重量%水溶液の粘度は、5,000mPa・sだった。
【0018】
結果を表1にまとめる。
【表1】
【0019】
コットンリンターパルプを用いた実施例1と比較例1の結果、コットンパルプを用いた実施例2と比較例2の結果より、本実施例では、粉砕動力原単位が低減され、粉砕によるパルプ中のセルロースの重合度低下の軽減、すなわち高粘性のセルロースエーテルを得られた。
【0020】
【発明の効果】
本発明の方法によれば、粉砕動力原単位が低減され、エネルギーを低下でき、粉砕によるパルプ中のセルロースの重合度低下が軽減し、すなわち高粘性のセルロースエーテルを得られる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a powdered pulp used for a raw material of cellulose ether and other industrial uses.
[0002]
[Prior art]
Powdered pulp is used for cellulose ether raw materials and other industrial purposes.
When trying to obtain a powdery pulp by pulverizing a sheet-like pulp, there has been no conventional technique that pays attention to the weight per unit area of the sheet-like pulp.
[0003]
[Problems to be solved by the present invention]
In the conventional technology, when the sheet pulp is pulverized, the pulverization power unit of the pulverizer is very large, and the degree of polymerization of cellulose, which is the main component of the pulp, is significantly reduced. The problem was that the viscosity of the aqueous solution of cellulose ether produced as a raw material was low.
An object of the present invention is to reduce the basic unit of pulverization power when pulverizing a sheet-like pulp to obtain a powdery pulp, and to reduce a decrease in the degree of polymerization of cellulose.
[0004]
[Means for Solving the Problems]
In order to solve the above-mentioned problems, the present invention controls the weight per area of the sheet-like pulp that is a pulverized raw material when the sheet-like pulp is pulverized to obtain a powdery pulp. Cotton linter pulp weight per surface area of 700~1200g / m 2 pulp sheet, wood pulp using a sheet-like pulp 900~1200g / m 2.
[0005]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, the present invention will be described in detail.
The cotton linter pulp of the present invention is a pulp obtained using fibers produced in cotton seeds as raw materials. The wood pulp of the present invention is a pulp obtained using wood as a raw material. The degree of polymerization of cellulose contained in cotton linter pulp and wood pulp is not limited, but usually those having a weight average degree of polymerization (hereinafter abbreviated as “Dpw”) by a viscosity measurement method of 500 to 8,000 are used.
[0006]
Pulp is classified into sheet pulp, powdered pulp, and cotton-like pulp based on its shape. The sheet-like pulp which is the object of the present invention is preferably a flat pulp having a thickness of 3 mm or less.
The manufacturing method of sheet pulp is not particularly limited.
[0007]
Sheet pulp usually contains about several to 10% by weight of water. The “weight per area” referred to in the present invention is a weight not including the weight of moisture. Although the weight per area apparently varies depending on the water content, the effect of the present invention is not affected if the water content is 10% by weight or less. That is, it is necessary to pay attention to the weight other than moisture.
The method for obtaining the weight per area excluding the weight of moisture is according to the following equation.
W = M × (1−0.01x) / S
Here, W is the weight per area excluding the weight of moisture, M is the weight of the sheet-like pulp with area S including moisture, and x is the moisture (% by weight) of this pulp. The moisture content of the pulp is measured by weight loss when 2 g of pulp pieces are dried at 105 ° C. for 1 hour or more.
[0008]
The area of the sheet-like pulp referred to in the present invention refers to the area of the largest surface among the six faces when a piece of sheet-like pulp is regarded as a hexahedron.
Cotton linter pulp used in the present invention, the weight per area of 650 g / m 2 or more, preferably sheet-like pulp 700~1,200g / m 2, wood pulp, 900 g / m 2 or more, preferably from 900 to 1 , 200 g / m 2 of sheet pulp. If it is smaller than that, the effect of the present invention, that is, the effect of reducing the power unit and the effect of reducing the polymerization degree may not be obtained.
The power unit is the required power of a pulp crusher for pulverizing a certain amount of sheet-like pulp to obtain a powdery pulp having a certain average particle diameter.
[0009]
The thickness and apparent density of the sheet-like pulp used in the present invention are not particularly limited, but usually those having a thickness of 0.5 to 2.5 mm and an apparent density of 0.4 to 1.0 g / ml are used. Since the weight per area can be expressed by the product of the thickness of the sheet and the apparent density, it is preferable to use a material having a larger apparent density if the thickness is constant and a material having a larger thickness if the apparent density is constant. Of course, the weight per area must satisfy 650 g / m 2 or more for cotton linter pulp and 900 g / m 2 or more for wood pulp.
[0010]
The sheet-like pulp used in the present invention can be made into an appropriate size and shape, for example, 0.5 to 2 cm square chips, which can be easily put into a pulverizer, according to the structure of the pulverizer before pulverization.
Examples of the pulverizer used in the pulverization of the present invention include a knife mill, an impact pulverizer, and a vertical roller mill, but are not particularly limited.
The average particle size of the powdered pulp obtained in the present invention is 1,000 μm or less, preferably 60 to 500 μm. When the average particle size exceeds 1,000 μm, the fluidity of the powdered pulp is lowered, and it may be difficult to handle as a powder.
[0011]
The cellulose ether of the present invention is prepared by a known method, for example, by adding an alkali cellulose such as sodium hydroxide or potassium hydroxide to powdered pulp, and then adding an etherifying agent such as methyl chloride, propylene oxide or ethylene oxide. Obtained by heating.
[0012]
【Example】
EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further in detail, this invention is not limited to description of these Examples.
Example 1
A sheet-like cotton linter pulp having a weight per area of 750 g / m 2 and a Dpw of 7,000 according to a cadoxene solution viscosity measurement method was pulverized with a knife mill (HA-2542: manufactured by Horai Iron Works). The grinding power unit was 0.17 kwh / kg. The average particle diameter of the obtained powdery pulp was 250 μm, and Dpw was 4,770.
100 parts by weight of the pulverized pulp was put into a reactor equipped with an internal stirrer, and after sufficient nitrogen substitution, 123 parts by weight of sodium hydroxide, 80 parts by weight of methyl chloride for methoxyl group substitution, and for substitution of hydroxypropoxyl group Add 21 parts by weight of propylene oxide, react at 40-100 ° C., purify with hot water until the residual salt content is about 1% by weight, and then dry to contain 1.2% by weight of water. A raw material hydroxypropylmethylcellulose was obtained. This raw material hydroxypropylmethylcellulose had a methoxyl substitution degree of 1.4 and a hydroxypropoxyl group substitution degree of 0.2. The degree of substitution indicates the number of substituents introduced per glucose unit. The viscosity of the obtained 1% by weight aqueous solution of hydroxypropylmethylcellulose was 19,000 mPa · s.
[0013]
Example 3
The same operation as in Example 1 was performed except that a sheet-like cotton linter pulp having a weight per area of 1200 g / m 2 was used. The pulverization power unit was 0.10 kwh / kg, the average particle size of the obtained powdered pulp was 250 μm, and Dpw was 4,850. The viscosity of a 1% by weight aqueous solution of hydroxypropylmethylcellulose was 19,500 mPa · s.
[0014]
Example 3
The same operation as in Example 1 was performed except that a sheet-like wood pulp having a weight per area of 950 g / m 2 and a Dpw of 4,000 was used. The basic unit of pulverization power was 0.13 kwh / kg, the average particle size of the obtained powdered pulp was 120 μm, and Dpw was 3,060. The viscosity of a 1% by weight aqueous solution of hydroxypropylmethylcellulose was 8,000 mPa · s.
[0015]
Example 4
The same operation as in Example 1 was performed except that a sheet-like wood pulp having a weight per area of 1,200 g / m 2 and a Dpw of 4,000 was used. The pulverization power basic unit was 0.10 kwh / kg, the average particle diameter of the obtained powdered pulp was 120 μm, and Dpw was 3,150. The viscosity of a 1% by weight aqueous solution of hydroxypropylmethylcellulose was 8,200 mPa · s.
[0016]
Comparative Example 1
The same operation as in Example 1 was performed except that a sheet-like cotton linter pulp having a weight per area of 570 g / m 2 was used. The basic unit of pulverization power is 0.25 kwh / kg, the average particle size of the obtained powdered pulp is 250 μm, Dpw is 4,500, and the viscosity of a 1% by weight aqueous solution of hydroxypropylmethylcellulose is 15,000 mPa · s. It was.
[0017]
Comparative Example 2
The same operation as in Example 1 was performed except that a sheet-like wood pulp having a weight per area of 750 g / m 2 was used. The basic unit of pulverization power is 0.17 kwh / kg, the average particle size of the obtained powdered pulp is 120 μm, Dpw is 2,390, and the viscosity of a 1 wt% aqueous solution of hydroxypropylmethylcellulose is 5,000 mPa · s. It was.
[0018]
The results are summarized in Table 1.
[Table 1]
[0019]
From the results of Example 1 and Comparative Example 1 using cotton linter pulp, and from the results of Example 2 and Comparative Example 2 using cotton pulp, in this example, the pulverization power basic unit is reduced, A reduction in the degree of polymerization of cellulose, that is, a highly viscous cellulose ether was obtained.
[0020]
【The invention's effect】
According to the method of the present invention, the basic unit of pulverization power can be reduced, energy can be reduced, and the decrease in the degree of polymerization of cellulose in the pulp due to pulverization can be reduced, that is, a highly viscous cellulose ether can be obtained.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000177875A JP4813640B2 (en) | 2000-06-14 | 2000-06-14 | Method for producing cellulose ether |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000177875A JP4813640B2 (en) | 2000-06-14 | 2000-06-14 | Method for producing cellulose ether |
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| JP2001354701A JP2001354701A (en) | 2001-12-25 |
| JP4813640B2 true JP4813640B2 (en) | 2011-11-09 |
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| JP2000177875A Expired - Lifetime JP4813640B2 (en) | 2000-06-14 | 2000-06-14 | Method for producing cellulose ether |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4581320B2 (en) * | 2002-09-27 | 2010-11-17 | 日本製紙株式会社 | Powdered cellulose and process for producing the same |
| CN101605816B (en) | 2007-02-16 | 2011-11-09 | 花王株式会社 | Process for producing noncrystalline cellulose |
| EP2075260A1 (en) | 2007-12-27 | 2009-07-01 | Shin-Etsu Chemical Co., Ltd. | Methods for preparing alkali cellulose and water-soluble cellulose ether |
| JP5252911B2 (en) | 2007-12-27 | 2013-07-31 | 信越化学工業株式会社 | Method for producing water-soluble cellulose ether |
| JP5503609B2 (en) | 2011-09-08 | 2014-05-28 | 信越化学工業株式会社 | Method for producing nonionic water-soluble cellulose ether |
| KR20200140196A (en) * | 2019-06-05 | 2020-12-15 | 신에쓰 가가꾸 고교 가부시끼가이샤 | Pulverized pulp and method of producing cellulose ether using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4241881A (en) * | 1979-07-12 | 1980-12-30 | Kimberly-Clark Corporation | Fiber separation from pulp sheet stacks |
| JPH02235901A (en) * | 1986-05-01 | 1990-09-18 | Dow Chem Co:The | Preparation of highly-viscous cellulose ether |
| JPH0791321B2 (en) * | 1987-07-22 | 1995-10-04 | ダイセル化学工業株式会社 | Method for producing cellulose acetate |
| JP2669555B2 (en) * | 1989-05-26 | 1997-10-29 | ダイセル化学工業株式会社 | Method for disintegrating cellulose sheet and method for producing cellulose acetate |
| JP2633042B2 (en) * | 1989-12-26 | 1997-07-23 | ダイセル化学工業株式会社 | Pulp sheet crushing method |
| JP2823944B2 (en) * | 1990-07-05 | 1998-11-11 | ダイセル化学工業株式会社 | Method for producing cellulose acetate |
| JP2999293B2 (en) * | 1991-07-02 | 2000-01-17 | ダイセル化学工業株式会社 | Method for producing cellulose acetate |
| JPH08245701A (en) * | 1995-03-08 | 1996-09-24 | Daicel Chem Ind Ltd | Highly transparent hydroxyalkyl cellulose and its production |
| JP3996653B2 (en) * | 1996-01-26 | 2007-10-24 | 信越化学工業株式会社 | Hydroxypropylcellulose with controlled substitution degree distribution |
| JP4028003B2 (en) * | 1996-05-31 | 2007-12-26 | 旭化成株式会社 | Method for preparing cellulose solution |
| JP4010345B2 (en) * | 1996-11-28 | 2007-11-21 | 信越化学工業株式会社 | Method for producing hydroxypropyl methylcellulose |
| JPH1121301A (en) * | 1997-07-03 | 1999-01-26 | Sumitomo Seika Chem Co Ltd | Production of hydroxypropylcellulose |
| JP2000007702A (en) * | 1998-06-23 | 2000-01-11 | Sumitomo Seika Chem Co Ltd | Preparation of hydroxypropyl cellulose |
| JP2001172893A (en) * | 1999-12-21 | 2001-06-26 | Sato Masako | Pulp sheet for forming deodorant product |
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2000
- 2000-06-14 JP JP2000177875A patent/JP4813640B2/en not_active Expired - Lifetime
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| JP2001354701A (en) | 2001-12-25 |
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