JPS62282097A - Continuous production of fire retardant pulp - Google Patents
Continuous production of fire retardant pulpInfo
- Publication number
- JPS62282097A JPS62282097A JP12354386A JP12354386A JPS62282097A JP S62282097 A JPS62282097 A JP S62282097A JP 12354386 A JP12354386 A JP 12354386A JP 12354386 A JP12354386 A JP 12354386A JP S62282097 A JPS62282097 A JP S62282097A
- Authority
- JP
- Japan
- Prior art keywords
- pulp
- urea
- reaction
- flame
- continuous production
- 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.)
- Pending
Links
- 239000003063 flame retardant Substances 0.000 title claims description 10
- 238000010924 continuous production Methods 0.000 title claims 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000000865 phosphorylative effect Effects 0.000 description 2
- 210000002700 urine Anatomy 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- LLDYDUXXNBDDFT-UHFFFAOYSA-N phosphoric acid urea Chemical compound NC(=O)N.P(=O)(O)(O)O.P(=O)(O)(O)O.P(=O)(O)(O)O LLDYDUXXNBDDFT-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000011345 viscous material Substances 0.000 description 1
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
３、発明の詳細な説明
［産業上の利用分野］
本発明は、難燃性パルプを量産化するのに適した連続製
造方法に関するものである。Detailed Description of the Invention 3. Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a continuous manufacturing method suitable for mass-producing flame-retardant pulp.
［従来の技術］
既に、燐酸化セルロースは難燃性パルプであることが知
られている。そしてこの燐酸化セルロースの製造方法も
いくつか知られている。[Prior Art] It is already known that phosphorylated cellulose is a flame-retardant pulp. Several methods for producing phosphorylated cellulose are also known.
その一つの方法は、綜合燐酸と尿素を含む反応液に原料
パルプを浸漬し、加圧脱水してから１００〜１１０℃で
約６０分乾燥し、次に１５０〜１６０℃で１５〜２０分
加熱反応させて燐酸化パルプを１ｑる方法が提案されて
いる（特願昭４９−４８６００号）。One method is to immerse the raw pulp in a reaction solution containing synthetic phosphoric acid and urea, dehydrate it under pressure, dry it at 100-110°C for about 60 minutes, and then heat it at 150-160°C for 15-20 minutes. A method of producing 1 q of phosphorylated pulp by reaction has been proposed (Japanese Patent Application No. 49-48600).
［発明が解決しようとする問題点］
前記した従来の製造方法は、乾燥を低温にて行い、反応
は高温で短時間に行い、２段階に分けてトータルで８０
分間必要としていた。[Problems to be solved by the invention] In the conventional production method described above, drying is carried out at a low temperature, reaction is carried out at a high temperature for a short time, and the process is divided into two stages for a total of 80
I needed a minute.
高温にて乾燥しない理由は、高温乾燥すると縮合燐酸（
反応液の主成分）中にｖ１離して存在する尿素が分解し
てパルプは空気酸化してしまい、パルプの繊維が結合力
を失っており、接着性のないバラバラのパルプになり、
紙が強度の弱いものになるからである。The reason why it doesn't dry at high temperatures is that when you dry at high temperatures, condensed phosphoric acid (
Urea, which is present at a distance of v1 in the main component of the reaction solution, decomposes and the pulp is oxidized in the air, causing the pulp fibers to lose their cohesive strength and become disjointed pulp with no adhesive properties.
This is because the paper becomes weaker.
したがってこのような堤象を避けるために、乾燥は極力
低温で、反応は短時間で行われることがしまりのある強
い紙を得るポイントである。Therefore, in order to avoid this phenomenon, drying should be carried out at as low a temperature as possible and the reaction should be carried out in a short period of time in order to obtain a tight and strong paper.
しかし、この従来の方法では余りに時間が掛かり過ぎて
現実的でない。製紙工場のスケールでは１日に１０を規
模の量産体制で検討すると莫大な設備費が掛かってしま
い、如何に燐酸化パルプの特性が認められても経済的に
不可能である。However, this conventional method is too time-consuming and impractical. On the scale of a paper mill, mass production of 10 units per day would require enormous equipment costs, making it economically impossible no matter how good the characteristics of phosphorylated pulp are.
若し乾燥、反応の全工程が数分の単位で可能となるなら
ば操業は連続的に、しかも極めて小さな設備で可能とな
るので燐酸化パルプのコストも大巾に下がることになり
、それに伴って需要は飛躍的に増加する。従って特に建
材関係で最近色々と問題になっている、火災と有毒ガス
の発生は、燐酸化パルプの使用によって解消できるもの
と期待されている。If the entire process of drying and reaction could be done in a few minutes, it would be possible to operate continuously and with extremely small equipment, which would greatly reduce the cost of phosphorylated pulp. Demand will increase dramatically. Therefore, it is expected that the use of phosphorylated pulp will solve the problems of fire and the generation of toxic gases, which have recently become a problem especially in relation to building materials.
［問題を解決するための手段］
この様な燐酸化パルプの製造に画期的な技術を開発する
ため研究中のところようや゛く解決できた。[Means for solving the problem] We were finally able to solve the problem while conducting research to develop a revolutionary technology for producing such phosphorylated pulp.
先ず燐酸化液に含まれる尿素の分解速度を遅くするため
の研究の結果、尿素の分解速度は、液のｐＨと密接なる
関係があることが判った。即ち、燐酸と尿素を混合し、
加熱することにより綜合燐酸が生成し、縮合度の上昇と
共にＩ）Ｈも上昇し最終的にはｐｉ−１８，５位になる
。そこで燐酸尿素の縮合課程、即ち混合しただけではｐ
Ｈｏ、ｓ位から加熱するに従って順次上昇するが、この
ｐＨの変化と尿素の分解の関係を検討した結果、ｌ）Ｈ
と尿素分解蓮度の関係が明らかになりＩ）Ｈ３〜７位の
ものが分解が遅く、しかも反応速度も速く、生成燐、酸
化パルプの物性も優れていることが分った。First, as a result of research into slowing down the decomposition rate of urea contained in a phosphorylating solution, it was found that the decomposition rate of urea is closely related to the pH of the solution. That is, by mixing phosphoric acid and urea,
By heating, synthesized phosphoric acid is produced, and as the degree of condensation increases, I)H also increases, eventually reaching the pi-18,5 position. Therefore, the condensation process of phosphoric acid urea, that is, the p
Ho increases sequentially as the temperature is heated from the s position, but as a result of examining the relationship between this pH change and the decomposition of urea, we found that l) H
The relationship between the degree of urea decomposition and the degree of urea decomposition was clarified, and it was found that I) H3-7 decomposition was slow, the reaction rate was fast, and the physical properties of the produced phosphorus and oxidized pulp were excellent.
一方、原料パルプに同−鉦の液を含浸してからのパルプ
の乾燥速度も同じ様なカーブであることが分った。On the other hand, it was found that the drying rate of the pulp after impregnating the raw material pulp with the same liquid had a similar curve.
またそ芯り低いｐＨ１以下のものも極端に遅いことが判
ったのである。It was also found that those with a low pH of 1 or less were also extremely slow.
その様な結果から燐酸と尿素を水に溶解し、加熱しＤＨ
３〜７位の混合液を用いる特願昭６１−０５５３０号発
明にＪ：る、難燃化液が高温乾燥に適し□ ていること
が判明した。Based on these results, phosphoric acid and urea were dissolved in water and heated to produce DH.
It has been found that the flame retardant liquid according to the invention of Japanese Patent Application No. 61-05530 using a mixed liquid of ranks 3 to 7 is suitable for high-temperature drying.
一方、乾燥、反応に対する加熱源として熱風を利用して
いるが、難燃化液の様に比較的粘調性のあるものを乾燥
するには、熱風よりも赤外線を使うのが理想的ではない
かと気付いて実験したところ予想以上の好結果が得られ
た。On the other hand, hot air is used as a heating source for drying and reactions, but it is not ideal to use infrared rays rather than hot air to dry relatively viscous materials such as flame retardant liquids. When I realized this and experimented, I got better results than I expected.
赤外線は電磁波の一種で物質に当ると吸収され、その物
質の分子や原子の固１有振動と吸収された赤外線の波長
が合って、共鳴を起こすことにより加熱するので゛ある
。Infrared rays are a type of electromagnetic waves that are absorbed when they hit a substance, and when the wavelength of the absorbed infrared rays matches the natural vibration of the molecules or atoms of the substance, they cause resonance and heat up.
従って熱風の様に物質の表面より徐々に熱伝導によって
加熱するものと違い内部より加熱するため乾燥速度が早
い。その結果赤外線によると、乾燥と反応とで僅か４〜
５分位で目的を達成できた。Therefore, unlike hot air, which gradually heats the material from the surface by thermal conduction, drying speed is faster because it heats from the inside. As a result, according to infrared rays, only 4~
I achieved my goal in about 5 minutes.
これは従来の熱風による場合と比較すると２０分の１位
の時間に短縮し、画期的なスピードである。また得られ
たパルプの特性も、数段秀れたものを得ることができる
。この様になったのも、反応液のｌ）Ｈを調節すること
と尿素の分゛解速度よりも早く乾燥反応の時間を短縮で
きた赤外線による加熱の結果である。This is an epoch-making speed that is about 1/20th the time compared to the conventional method using hot air. Furthermore, the properties of the obtained pulp can be improved by several orders of magnitude. This result was also a result of adjusting the l)H of the reaction solution and heating with infrared rays, which made it possible to shorten the drying reaction time faster than the decomposition rate of urea.
［実施例１］ ’
燐ＩＩ（１００％換算） １モル １００グラム尿″
素 ３モル １８０グラム水
３００グラム以上のものを加熱し
て縮合反応を行った。[Example 1] 'Phosphorus II (100% conversion) 1 mole 100 grams urine''
3 moles 180 grams water
A condensation reaction was carried out by heating 300 grams or more.
ｐｌ−１８近くになると発熱反応によって液□が固化し
、その結果約２３０グラムの綜合燐酸の固形物が得られ
た。At near pl-18, the liquid □ solidified due to an exothermic reaction, resulting in approximately 230 grams of solid phosphoric acid.
それを水６００グラム、尿素１２０グラムの溶液に溶解
して燐酸化液（ｐＨ８，４）とした（薬品１１１度３９
％）。It was dissolved in a solution of 600 grams of water and 120 grams of urea to make a phosphorylating solution (pH 8.4) (chemicals 111 degrees, 39 degrees).
%).
これに乾燥パルプシートを３０秒ＩＩ浸漬し、そのま）
圧縮脱水したものを１１０℃の恒温乾燥器で６０分間乾
燥し、更に１５５℃の恒温乾燥器で１８分間反応させた
。Dip the dry pulp sheet in this for 30 seconds (II)
The compressed and dehydrated product was dried in a constant temperature dryer at 110°C for 60 minutes, and further reacted for 18 minutes in a constant temperature dryer at 155°C.
次に常法（Ｊ Ｉ Ｓ Ｐ８２０９）によりシートし
て紙力、燐の定量した。Next, the paper was sheeted using a conventional method (JIS P8209), and the paper strength and phosphorus content were determined.
［実施例２］ ・・
燐酸（１００％換算） １モル １ｆｌＯダラム尿
・−素 ３モル １８０グラム−水
３０Ｇグラム以上のものを加熱し
、（１）’ｐＨ２，１、（２）−６＝
吋１３４、（３） １１１１−１ ４．１、（４＞
ｐＨ５，８のものを４種調整した。[Example 2] Phosphoric acid (100% conversion) 1 mol 1 flO Durum urine
- element 3 moles 180 grams - water
Heating 30G grams or more, (1)'pH2,1, (2)-6= 吋134, (3) 1111-1 4.1, (4>
Four types of pH 5 and 8 were prepared.
それぞれの液に、尿素１２０グラムと水を加えて全体の
液をｉ、ｏｏｏグラムとなる様に調整した（薬品ｍ度４
０％）。To each solution, 120 grams of urea and water were added to adjust the total solution to i, ooo grams (chemical m degree 4
0%).
調整後の液に乾燥パルプシートを実施例１と同じ条件で
浸漬し、脱水し、次に直ちに赤外線にて３分以上加熱し
たものを実施例１と同様にシートし、強度、燐の定量を
おこなった。A dry pulp sheet was immersed in the adjusted solution under the same conditions as in Example 1, dehydrated, and then immediately heated with infrared rays for 3 minutes or more.The sheet was then sheeted in the same manner as in Example 1, and the strength and phosphorus content were determined. I did it.
１ 酸イパルプの 化
加熱源 乾燥 反応 合計 燐結合１１０℃
１５５℃
熱風 ６０分 １８分 ７８分 ６．５
％赤外線 １）Ｈ
（１） ２．１ ４分２０秒 ５．１
％（２） ３．４ ５．９（３
） ４．１ ６
．３（４） ５．８
６．７２ 千Ｐ の２
坪量２う１引張り裁 引裂会う ■
熱風 ６０ ３．５ ４６
小赤外線
（１） ６０ ４．９ ２４大
（２） ６０ ６．１ ３［３中
（３） ６０ ７．３ ２０小
（４，） ｅｏ ７．６１４小
■ＪＩＳ Ｐ８１１３ ■ＪＩＳ Ｐ８１１（３
■肉眼［発明の効果］
本発明の製造方法によれば、乾燥と加熱が連続して行え
るので非常に短時間で難燃性パルプを製造できるので量
産に適している。1 Acid pulp chemical heating source Drying reaction Total phosphorus bond 110℃
155℃ hot air 60 minutes 18 minutes 78 minutes 6.5
% Infrared 1) H (1) 2.1 4 minutes 20 seconds 5.1
%(2) 3.4 5.9(3
) 4.1 6
．． 3 (4) 5.8
6.72 1,000P 2 Basis weight 2 1 Tensile cut Tear ■ Hot air 60 3.5 46
Small infrared (1) 60 4.9 24 large (2) 60 6.1 3 [3 medium (3) 60 7.3 20 small (4,) eo 7.614 small ■JIS P8113 ■JIS P811 (3
■Macroscopically [Effects of the Invention] According to the production method of the present invention, drying and heating can be carried out continuously, so flame-retardant pulp can be produced in a very short time, making it suitable for mass production.
同時に反応が短時間で行われるため品質の秀れた燐酸化
パルプを得ることができる。At the same time, since the reaction is carried out in a short time, it is possible to obtain phosphorylated pulp of excellent quality.
Claims (2)
、乾燥、反応を連続して行う難燃性パルプの連続製造方
法。(1) A method for continuous production of flame-retardant pulp, in which a pulp sheet is immersed in a flame-retardant liquid and then dehydrated, dried, and reacted continuously.
り、乾燥、反応を赤外線を用いて行うところの請求の範
囲（１）に請求の難燃性パルプの連続製造方法。(2) The method for continuously producing flame-retardant pulp as claimed in claim (1), wherein the flame-retardant liquid is a mixture of phosphoric acid and urea dissolved in water, and the drying and reaction are performed using infrared rays.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12354386A JPS62282097A (en) | 1986-05-30 | 1986-05-30 | Continuous production of fire retardant pulp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12354386A JPS62282097A (en) | 1986-05-30 | 1986-05-30 | Continuous production of fire retardant pulp |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62282097A true JPS62282097A (en) | 1987-12-07 |
Family
ID=14863196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12354386A Pending JPS62282097A (en) | 1986-05-30 | 1986-05-30 | Continuous production of fire retardant pulp |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62282097A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012149360A (en) * | 2011-01-19 | 2012-08-09 | Kurabo Ind Ltd | Moisture-absorbing heat-generating cellulose fiber fabric and method for manufacturing the same |
-
1986
- 1986-05-30 JP JP12354386A patent/JPS62282097A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012149360A (en) * | 2011-01-19 | 2012-08-09 | Kurabo Ind Ltd | Moisture-absorbing heat-generating cellulose fiber fabric and method for manufacturing the same |
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