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JPS626040B2 - - Google Patents
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JPS626040B2 - - Google Patents

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Publication number
JPS626040B2
JPS626040B2 JP53047077A JP4707778A JPS626040B2 JP S626040 B2 JPS626040 B2 JP S626040B2 JP 53047077 A JP53047077 A JP 53047077A JP 4707778 A JP4707778 A JP 4707778A JP S626040 B2 JPS626040 B2 JP S626040B2
Authority
JP
Japan
Prior art keywords
sulfate
manufacturing
alum
cellulose
polyvalent metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
JP53047077A
Other languages
Japanese (ja)
Other versions
JPS54138060A (en
Inventor
Shigenori Ichikawa
Satoshi Wada
Shuji Masuda
Tetsuo Hasegawa
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Otsuka Chemical Co Ltd
Original Assignee
Otsuka Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Otsuka Chemical Co Ltd filed Critical Otsuka Chemical Co Ltd
Priority to JP4707778A priority Critical patent/JPS54138060A/en
Publication of JPS54138060A publication Critical patent/JPS54138060A/en
Publication of JPS626040B2 publication Critical patent/JPS626040B2/ja
Granted legal-status Critical Current

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Description

【発明の詳細な説明】[Detailed description of the invention]

本発明はセルロース繊維板の製造法に関する。 従来のセルロース繊維板は高比重で密度が高
く、いまだ低密度で連続微空孔を有する難燃性セ
ルロース繊維板は得られていない。低密度で連続
微空孔を有するセルロース繊維板にすることによ
つて断熱性および吸音性の良好な繊維板が得られ
る。又難燃性とするためには抄造成形後、難燃剤
を含浸又はスプレー等の方法で行うことによつて
処理されている。しかしこのような方法ではセル
ロース繊維板に難燃剤が物理的に付着するのみ
か、化学的に結合したとしても一部分のみしか結
合していないのが通常である。従つてこれらの方
法で行つた場合塗付した難燃剤が経時的に白華現
象、吸湿性、薬剤公害ならびに難燃性の低下等の
問題を生じ、充分満足できる難燃性セルロース繊
維は得られていない。 本発明者は上記の欠点を解決すべく、鋭意研究
の結果、あらかじめ木材パルプを低縮合リン酸ア
ンモニウム水溶液で処理乾燥した難燃性リン酸セ
ルロースに多価金属塩を反応させ、酸性条件で抄
造成形後乾燥することによつて従来にない低密度
で嵩高い連続微空孔を有する難燃性低密度セルロ
ース繊維板の製造を可能にし得たのである。 本発明の詳細について説明すると、リン酸セル
ロースは木材パルプに低縮合リン酸アンモニウム
水溶液を含浸させた後に乾燥し、更に130℃〜170
℃の温度でエステル化することによつて製造でき
る。得られたリン酸セルロースを水に対し約2.5
重量%の濃度でビーター離解し、パルプスラリー
とする。次に多価金属塩の溶液を用い、PH2.0〜
7.0に、好ましくは2.7〜6.5に調整する。PHが2.0
より低い場合セルロースの膨潤が起こらず、PHが
7.0を越える場合抄造が困難となる。PH調整後抄
造成形機を用い繊維板に成形し、吸引脱水を行
い、水分含有率70%程度の繊維板とし、100〜125
℃で1〜3時間通風乾燥する。 ここで用いられる多価金属塩としては硫酸アル
ミニウム、硫酸第2鉄、硫酸第1鉄、硫酸亜鉛、
硫酸銅、硫酸ニツケル、硫酸マンガン、硫酸マグ
ネシウム、アルミニウムミヨウバン、鉄ミヨウバ
ン、ナトリウムミヨウバン、カリウムミヨウバ
ン、クロムミヨウバン、モール塩、塩化第2鉄、
塩化アルミニウム、塩化亜鉛等である。この多価
金属塩の中で特に好ましい塩は硫酸アルミニウ
ム、硫酸第2鉄、アルミニウムミヨウバン、鉄ミ
ヨウバン、塩化亜鉛である。これら多価金属塩は
通常20〜40重量%の溶液として用いるのが好まし
い。これらの多価金属塩はリン酸セルロース繊維
スラリーのPHを調整すると同時に、セルロースに
結合しているリン酸基に金属が結合してセルロー
スの繊維束の嵩を増大させるため、低密度の繊維
束が得られ、抄造、乾燥した繊維板が得られるも
のと考えられる。 このようにして得られたリン酸セルロース繊維
板は未処理のセルロース繊維板に比較して1.5〜
7.0倍の嵩をもつた繊維板が得られ、しかも連続
微空孔を有するため断熱性、吸音性および結露防
止効果をもつた繊維板となり、また同時に繊維板
に抄造成型する前にあらかじめ、化学的結合によ
る難燃化処理が行われているため、経時的にも難
燃剤による白華現象、吸湿性、薬剤公害ならびに
難燃性低下等の起きない繊維板が得られるので、
吸音材、断熱材ならびに緩衝材として有効に用い
られ、この繊維板はJIS A 1321の難燃三級にも
合格するものである。 以下に本発明を明らかにするために実施例を示
す。 実施例 1 NBKPパルプ100gを縮合ポリリン酸アンモニ
ウムを主体とした難燃剤(大塚化学薬品株式会社
製、商品名FR−30)150gに充分に浸漬した後、
付着難燃剤を除去し、80〜90℃で1時間乾燥す
る。更に充分にエステル化を行うために140℃で
25分間空気浴中で反応させリン酸セルロース繊維
120gを得た。得られたリン酸セルロース500g
〔Canadian Standard Freeness、CSF(水
性)=720ml〕を水20に加えビーター離解し、約
2Kgを単位としたリン酸セルローススラリーに硫
酸アルミニウム、30重量%水溶液を用いPHを2.7
〜6.5に調整処理後、充分分散を行い、抄造機で
350×650mmに成形し繊維板を得た。この繊維板を
吸引脱水し水分含有率70%とした繊維板を100〜
125℃で通気乾燥し目的とする繊維板を得た。尚
対照として無処理のNBKPパルプを用いて同条件
で処理し、繊維板を得た。それぞれの繊維板の厚
さならびに密度の測定結果を下記第1表に示す。
The present invention relates to a method for manufacturing cellulose fiberboard. Conventional cellulose fiberboards have high specific gravity and high density, and flame-retardant cellulose fiberboards with low density and continuous micropores have not yet been obtained. By making a cellulose fiberboard with low density and continuous micropores, a fiberboard with good heat insulation and sound absorption properties can be obtained. In order to make it flame retardant, it is treated by impregnating or spraying with a flame retardant after paper forming. However, in such a method, the flame retardant is usually only physically attached to the cellulose fiberboard, or even if it is chemically bonded, it is only partially bonded. Therefore, when these methods are used, the applied flame retardant causes problems such as efflorescence, hygroscopicity, chemical pollution, and a decrease in flame retardancy over time, making it impossible to obtain sufficiently flame-retardant cellulose fibers. Not yet. In order to solve the above-mentioned drawbacks, as a result of intensive research, the present inventors reacted a polyvalent metal salt to flame-retardant cellulose phosphate, which had been prepared by treating wood pulp with a low-condensed ammonium phosphate aqueous solution and dried it, and produced paper under acidic conditions. By drying after molding, it became possible to produce a flame-retardant low-density cellulose fiberboard with unprecedentedly low density and bulky continuous micropores. To explain the details of the present invention, cellulose phosphate is produced by impregnating wood pulp with a low condensed ammonium phosphate aqueous solution and then drying it at 130°C to 170°C.
It can be produced by esterification at a temperature of °C. The obtained cellulose phosphate is mixed with water at a rate of about 2.5
Disintegrate with a beater at a concentration of % by weight to obtain pulp slurry. Next, using a solution of polyvalent metal salt, PH2.0~
Adjust to 7.0, preferably 2.7 to 6.5. PH is 2.0
If the pH is lower, no swelling of cellulose occurs and the pH is
If it exceeds 7.0, papermaking becomes difficult. After adjusting the pH, it is formed into a fiberboard using a paper forming machine, and dehydrated by suction to make a fiberboard with a moisture content of about 70%.
Air dry at ℃ for 1-3 hours. The polyvalent metal salts used here include aluminum sulfate, ferric sulfate, ferrous sulfate, zinc sulfate,
Copper sulfate, nickel sulfate, manganese sulfate, magnesium sulfate, aluminum alum, iron alum, sodium alum, potassium alum, chromium alum, Mohr's salt, ferric chloride,
These include aluminum chloride and zinc chloride. Among these polyvalent metal salts, particularly preferred are aluminum sulfate, ferric sulfate, aluminum alum, iron alum, and zinc chloride. It is usually preferable to use these polyvalent metal salts as a 20 to 40% by weight solution. These polyvalent metal salts adjust the pH of the cellulose phosphate fiber slurry, and at the same time, the metal binds to the phosphate groups bonded to cellulose and increases the bulk of the cellulose fiber bundle, resulting in a low-density fiber bundle. It is thought that a paper-made and dried fiberboard can be obtained. The cellulose phosphate fiberboard obtained in this way has a 1.5 to
A fiberboard with 7.0 times the bulk can be obtained, and since it has continuous micropores, it has heat insulation, sound absorption, and dew condensation prevention effects. Because flame retardant treatment is carried out through chemical bonding, fiberboard can be obtained that does not suffer from efflorescence, hygroscopicity, chemical pollution, or deterioration of flame retardancy caused by flame retardants over time.
It is effectively used as a sound absorbing material, a heat insulating material, and a cushioning material, and this fiberboard also passes JIS A 1321 flame retardant class 3. Examples are shown below to clarify the present invention. Example 1 After fully immersing 100 g of NBKP pulp in 150 g of a flame retardant mainly composed of condensed ammonium polyphosphate (manufactured by Otsuka Chemical Co., Ltd., trade name FR-30),
Remove the adhering flame retardant and dry at 80-90°C for 1 hour. At 140℃ to further perform esterification.
Phosphate cellulose fibers reacted in an air bath for 25 min
Obtained 120g. 500g of cellulose phosphate obtained
[Canadian Standard Freeness, CSF (aqueous) = 720 ml] was added to 20 ml of water and disintegrated with a beater, and the pH was adjusted to 2.7 using aluminum sulfate and a 30% by weight aqueous solution to the phosphate cellulose slurry in units of about 2 kg.
After adjusting to ~6.5, thoroughly disperse and process using a paper making machine.
A fiberboard was obtained by molding to 350 x 650 mm. This fiberboard is dehydrated by suction and the moisture content is 70%.
The target fiberboard was obtained by air drying at 125°C. As a control, untreated NBKP pulp was treated under the same conditions to obtain a fiberboard. The measurement results of the thickness and density of each fiberboard are shown in Table 1 below.

【表】【table】

【表】 実施例 2 実施例1の硫酸アルミニウムをアルミニウムミ
ヨウバンに代えて他は同様にして得たセルロース
繊維板の測定結果を下記第2表に示す。
[Table] Example 2 The measurement results of a cellulose fiber board obtained in the same manner as in Example 1 except that aluminum sulfate was replaced with aluminum alum are shown in Table 2 below.

【表】 実施例 3 実施例1の硫酸アルミニウムを塩化亜鉛に代え
て他は同様にして得たセルロース繊維板の測定結
果を下記第3表に示す。
[Table] Example 3 The measurement results of a cellulose fiber board obtained in the same manner as in Example 1 except that aluminum sulfate was replaced with zinc chloride are shown in Table 3 below.

【表】 Γ難燃性試験 実施例1で得た繊維板をJIS A 1321の難燃性
試験方法に基づき難燃性試験を行つた結果を下記
第4表に示す。
[Table] Γ Flame Retardancy Test The fiberboard obtained in Example 1 was subjected to a flame retardancy test based on the JIS A 1321 flame retardancy test method, and the results are shown in Table 4 below.

【表】【table】

【表】【table】

Claims (1)

【特許請求の範囲】 1 りん酸セルロースを水中にて離解しパルプス
ラリー状とした後に、多価金属塩を作用させ、酸
性条件にて抄造成形し乾燥することを特徴とする
難燃性低密度セルロース繊維板の製造法。 2 りん酸セルロースが、木材パルプを低縮合り
ん酸アンモニウム水溶液に含浸させた後に乾燥
し、更に130〜170℃の温度でエステル化して得ら
れたものである特許請求の範囲第1項に記載の製
造法。 3 多価金属塩が硫酸アルミニウム、硫酸第2
鉄、硫酸第1鉄、硫酸亜鉛、硫酸銅、硫酸ニツケ
ル、硫酸マンガン、硫酸マグネシウム、アルミニ
ウムミヨウバン、鉄ミヨウバン、ナトリウムミヨ
ウバン、カリウムミヨウバン、クロムミヨウバ
ン、モール塩、塩化第2鉄、塩化アルミニウム、
塩化亜鉛である特許請求の範囲第1項に記載の製
造法。 4 酸性条件が多価金属塩と作用したパルプスラ
リーのPHが2.0〜7.0の範囲である特許請求の範囲
第1項に記載の製造法。 5 PHが2.7〜6.5の範囲である特許請求の範囲第
4項に記載の製造法。 6 抄造成形後の乾燥温度が100〜125℃である特
許請求の範囲第1項に記載の製造法。
[Claims] 1. A flame-retardant low-density product characterized in that cellulose phosphate is disintegrated in water to form a pulp slurry, then treated with a polyvalent metal salt, formed into a paper under acidic conditions, and dried. Method for manufacturing cellulose fiberboard. 2. Cellulose phosphate according to claim 1, wherein the cellulose phosphate is obtained by impregnating wood pulp with a low condensed ammonium phosphate aqueous solution, drying it, and further esterifying it at a temperature of 130 to 170°C. Manufacturing method. 3 The polyvalent metal salt is aluminum sulfate, secondary sulfate
Iron, ferrous sulfate, zinc sulfate, copper sulfate, nickel sulfate, manganese sulfate, magnesium sulfate, aluminum alum, iron alum, sodium alum, potassium alum, chromium alum, Mohr's salt, ferric chloride, chloride aluminum,
The manufacturing method according to claim 1, which is zinc chloride. 4. The manufacturing method according to claim 1, wherein the pH of the pulp slurry treated with the polyvalent metal salt under acidic conditions is in the range of 2.0 to 7.0. 5. The manufacturing method according to claim 4, wherein the PH is in the range of 2.7 to 6.5. 6. The manufacturing method according to claim 1, wherein the drying temperature after paper forming is 100 to 125°C.
JP4707778A 1978-04-19 1978-04-19 Manufacturing of flame retardant low-density cellulosic fiber board Granted JPS54138060A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP4707778A JPS54138060A (en) 1978-04-19 1978-04-19 Manufacturing of flame retardant low-density cellulosic fiber board

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4707778A JPS54138060A (en) 1978-04-19 1978-04-19 Manufacturing of flame retardant low-density cellulosic fiber board

Publications (2)

Publication Number Publication Date
JPS54138060A JPS54138060A (en) 1979-10-26
JPS626040B2 true JPS626040B2 (en) 1987-02-07

Family

ID=12765098

Family Applications (1)

Application Number Title Priority Date Filing Date
JP4707778A Granted JPS54138060A (en) 1978-04-19 1978-04-19 Manufacturing of flame retardant low-density cellulosic fiber board

Country Status (1)

Country Link
JP (1) JPS54138060A (en)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002044305A2 (en) 2000-11-28 2002-06-06 Astaris Llc Fire retardant compositions with reduced aluminum corrosivity
US6780991B2 (en) 2000-11-28 2004-08-24 Astaris Llc Biopolymer thickened fire retardant compositions
US6802994B1 (en) * 2000-11-28 2004-10-12 Astaris Llc Fire retardant compositions containing ammonium polyphosphate and iron additives for corrosion inhibition
US6846437B2 (en) * 2000-11-28 2005-01-25 Astaris, Llc Ammonium polyphosphate solutions containing multi-functional phosphonate corrosion inhibitors
WO2005047599A2 (en) 2003-11-08 2005-05-26 Lally Thomas J Method for manufacturing fire-retardant cellulose-based materials
US8425717B2 (en) * 2010-02-09 2013-04-23 Latitude 18, Inc. Phosphate bonded composites and methods
SE538956C2 (en) * 2015-05-22 2017-03-07 Innventia Ab Use of a paper or paperboard product as a middle layer in a paperboard
JP6558421B2 (en) * 2017-10-24 2019-08-14 王子ホールディングス株式会社 Cellulose sheet

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS49108309A (en) * 1973-02-22 1974-10-15
JPS607677B2 (en) * 1975-12-30 1985-02-26 古河電気工業株式会社 Flame-retardant smoke-proofing agent with improved pot life

Also Published As

Publication number Publication date
JPS54138060A (en) 1979-10-26

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