CN1034938A - The preparation of expansion cellulose sponge - Google Patents
The preparation of expansion cellulose sponge Download PDFInfo
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- CN1034938A CN1034938A CN 88105466 CN88105466A CN1034938A CN 1034938 A CN1034938 A CN 1034938A CN 88105466 CN88105466 CN 88105466 CN 88105466 A CN88105466 A CN 88105466A CN 1034938 A CN1034938 A CN 1034938A
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Abstract
The present invention is the preparation of expansion cellulose sponge, belongs to organic high molecular compound.It is that immersion makes corresponding soda cellulose in 22%, 2% sodium hydroxide solution respectively, above-mentioned soda cellulose places the commentaries on classics still to carry out the vacuum sulfonation in the lump with pulp, Limonene fiber crops, use molten Jie of diluted sodium hydroxide solution then, when having made required viscose glue, the Limonene fiber crops are evenly dispersed among the viscose glue.Above-mentioned viscose glue and saltcake is mixed, successively adopt alternating-current, the heating of saltcake saturated solution, make expansion cellulose sponge with certain physical strength.The cavernous body of compressed slabbing is met inflatable 10 to 15 times of water 10 seconds.
Description
The invention relates to the preparation of expansion cellulose Sponge, and a kind of more practical preparation method who improves Mierocrystalline cellulose Sponge physical strength.
The Mierocrystalline cellulose Sponge is normally mixed with viscose glue, fortifying fibre and pore-creating agent, injects mould, makes viscose ripening, regeneration and makes through heating.Pore-creating agent is melted in maturation, regenerative process or molten Jie, causes the formation in Sponge hole, and the effect of fortifying fibre is the physical strength that improves Sponge.
In order to improve the physical strength of Sponge, at first be to need fortifying fibre is evenly dispersed among the viscose glue, secondly be to make between the regenerated cellulose of fortifying fibre and formation Sponge good adhesiveproperties is arranged.Yet, the general natural reinforcing fiber element that adopts, poor to the viscose solution affinity, natural reinforcing fiber is difficult to be evenly dispersed in the viscose solution, and the gathering and the caking phenomenon of fortifying fibre very easily takes place in the process of sneaking into.
At above-mentioned situation, people have adopted and added wetting agent or dispersion agent in viscose solutions, to improve the wetting property of natural reinforcing fiber in viscose solution, reach the purpose of homodisperse.Yet, because the mentioned reagent costliness, effect is not good enough, so should not adopt; Thereafter, USP 3,131, and 076 has proposed with free alkali to 9～12% in the strong caustic adjusting viscose solution, and natural reinforcing fiber places above-mentioned solution, and swelling, sulfonation subsequently take place, thereby reaches the purpose of homodisperse.But this process need consume a large amount of sodium hydroxide, after Sponge generates, faces again and handles excessive sodium hydroxide, so this method has not only increased interpolation sodium hydroxide and fiber swollen technological process, having improved unit consumption and cost, increased three wastes processing again, is to be unfavorable for suitability for industrialized production.
As everyone knows, the hydroxyl in the Mierocrystalline cellulose glucose unit of natural fiber (cotton, flax, jute He Limonene fiber crops etc.) is replaced by sodium sulfonate, then can improve its molten Jie's performance in diluted sodium hydroxide solution significantly.The present invention then adopts this principle, natural reinforcing fiber is carried out sulfonating surface handle, improve its wetting property in viscose solution, thereby is situated between natural reinforcing fiber uniformly dispersed in viscose solution of having determined; Meanwhile, because the good sulfonation on natural reinforcing fiber surface, in its component and the viscose solution sodium cellulose xanghate real be consistent, so form the regenerated cellulose and the natural reinforcing fiber of Sponge good adhesiveproperties is arranged, the Sponge of gained then has good physical strength.
Technological process of the present invention is: the sodium hydroxide solution with different concns carries out alkaline purification to pulp and natural reinforcing fiber, makes corresponding soda cellulose.The soda cellulose of above-mentioned gained places in the sulfonation still in the lump, adds dithiocarbonic anhydride and carries out the vacuum sulfonation reaction.Reaction finishes pulp and has obtained abundant sulfonation, and the top layer sulfonation only takes place natural reinforcing fiber.Therefore, when with diluted sodium hydroxide solution molten Jie, make have high gamma value viscose solution in, natural reinforcing fiber also is evenly dispersed among the viscose solution.Above-mentioned viscose solution and pore-creating agent is mixed, make viscose ripening and regeneration through heating, can make expansion cellulose Sponge with good mechanical strength.
Therefore, main purpose of the present invention provides a kind of natural reinforcing fiber that makes and is dispersed in the viscose solution evenly, apace, the simple and easy and practical method for preparing the required slurry of expansion cellulose Sponge.
Another object of the present invention is to get rid of to add strong caustic and fiber swollen technological process in viscose solution, thereby has reduced raw-material unit consumption and production cost, reduces the corresponding three wastes and handles.
The required pulp of preparation viscose glue can be a wood pulp, can also be linters, wherein is advisable with linters especially.The concentration of sodium hydroxide solution that pulp is carried out the alkali immersion is 18～22%; Temperature is 20 ℃; Time is 1-2 hour; Thereafter press ratio is controlled at 2.8～3.0.
Adopt natural reinforcing fiber to be: cotton, jute, flax He Limonene fiber crops etc., wherein You Yi Limonene fiber crops are advisable.The concentration of sodium hydroxide solution that natural reinforcing fiber is carried out the alkali immersion is 1～10%, and more desirable concentration of sodium hydroxide solution is 2～6%; Temperature is 20 ℃; Time is 10～30 minutes, and more desirable soak time is 10～15 minutes; Thereafter press ratio is controlled at 2.8～3.0.The consumption of natural reinforcing fiber is 2.5～15% of a pulp consumption.
The above-mentioned soda cellulose that makes is placed in the sulfonation still after crushed, and the amount that adds dithiocarbonic anhydride is 30～60% of a pulp consumption; Temperature of reaction is controlled at 15～35 ℃; Time is to carry out the vacuum sulfonation reaction in 1～2 hour.The sodium cellulose xanghate that reaction finishes gained is dissolved in 1～5% the sodium hydroxide solution, and particularly desirable concentration of sodium hydroxide solution is 2～4%; Make in the viscose solution content of cellulose and be advisable with 5～9%, particularly desirable content of cellulose is 6～7%.
The pore-creating agent of above-mentioned employing can be a sodium sulfate, and is wherein more desirable with saltcake especially.Its consumption is 3～6 times of viscose glue consumption, is advisable with 5～6 times especially.
With above-mentioned viscose solution and pore-creating agent fully mixed after, place both sides to have in the heating tank of battery lead plate, at first adopt the 50HZ alternating-current to heat up, treat most molten Jie of saltcake pore-creating agent or fusion after, it is moved in the saturated solution groove of saltcake, continue to heat up, till viscose glue holomorphosis.With the Sponge of hot wash gained, clean residual saltcake and sodium hydroxide, make required expansion cellulose Sponge through drying, vacuum-drying, compression and cutting afterwards.
The Sponge that is made by aforesaid method has good expansion character, and the Sponge of compressed slabbing is met in the water 10 seconds inflatable 10～15 times, and kept excellent mechanical intensity.If spray the fire-retardant aqueous solution to Sponge, have same expansion character, after And was to be dried, this sponge physical efficiency reached from fire from the flame retardant effect that puts out.
Expansion cellulose Sponge of the present invention is the seal construction material that cable passes through deck or floor, also can be used as industry, civilian scrubbing tool, and its range of application is at U.S.P2, has made detailed description in 295823.
Other purposes of the present invention are illustrated in example, but patent right requires not to be subjected to the restriction of example.
" example "
(special 0.5～1.0cm) places respectively in the immersion slot of 22% and 5% sodium hydroxide solution with 40g cotton linter dissolving pulp and 2g Limonene fiber crops, soaked 1 hour and 10 minutes at 20 ℃, superfluous sodium hydroxide solution is removed in extruding then, and its pressure ratio is controlled at 2.8～3.0.Alkali fiber after the squeezing places 2 in the lump through pulverizing
lThe stainless steel hexagonal change in the still, open vacuum pump, treat that vacuum tightness reaches 700mmHg/cm
2More than, adding 20g dithiocarbonic anhydride and carry out the vacuum sulfonation reaction, temperature of reaction rises to 35 ℃ gradually by room temperature, and the reaction times is 2 hours.Sulfonation reaction finishes to make required viscose solution with above-mentioned sodium cellulose xanghate of molten Jie of 4% sodium hydroxide solution 550ml and natural reinforcing fiber, and meanwhile natural reinforcing fiber also is evenly dispersed among the viscose solution.
Weigh above-mentioned viscose solution 60g and saltcake 3000g, mixedly be placed on both sides and have in the heating tank of battery lead plate through fully stirring, the alternating-current that applies 50HZ between two electrodes heats, make feed temperature rise to 55 ℃ gradually, 55～70 ℃ of insulations 30 minutes, after treating that most saltcake is by molten Jie and fusion, during the Sponge basic forming, it is changed in another groove that fills saturated saltcake solution, continuing to be heated to 85 ℃ of And is incubated more than 30 minutes, till viscose glue holomorphosis at 85～95 ℃.Reaction finishes the back taking-up and removes residual saltcake and a spot of sodium hydroxide in the Sponge with 80～100 ℃ of washings, dries and place vacuum oven, is compressed into the thick sheet of 5～6mm thereafter, cuts into required size, deposits with standby under drying conditions.
The above-mentioned Sponge that makes, contain the fire-retardant aqueous solution of borax, Sodium Tetraborate and sodium phosphate through spray after, can expand rapidly.And has certain flame retardant properties after drying, reach from fire from putting out.Even Sponge does not give off poisonous gas when burning.
Claims (11)
1, a kind of comprising with viscose glue, natural reinforcing fiber and pore-creating agent, through mixing, heat the method that maturation and regeneration prepare the expansion cellulose Sponge, it is characterized in that: the sodium hydroxide solution with lower concentration soaks natural reinforcing fiber, carry out the vacuum sulfonation in the lump with the soda cellulose of pulp gained, thereafter the sodium hydroxide solution with lower concentration carries out molten Jie to above-mentioned sodium cellulose xanghate, when making required viscose, natural reinforcing fiber is evenly dispersed among the viscose solution.
2, be cotton, jute, flax He Limonene fiber crops by the described natural reinforcing fiber of claim 1.
3, by claim 1,2 described natural reinforcing fiber Shi Limonene fiber crops.
4, be 2.5～15% of pulp consumption by the described natural reinforcing fiber consumption of claim 1.
5, described natural reinforcing fiber is carried out the concentration that low-concentration sodium hydroxide solution soaks is 1～10% by claim 1.
6, by claim 1,5 described natural reinforcing fiber is carried out the concentration that low-concentration sodium hydroxide solution soaks is 2～6%.
7, described natural reinforcing fiber is carried out the time that low-concentration sodium hydroxide solution soaks is 10～30 minutes by claim 1.
8, by claim 1,7 described natural reinforcing fiber is carried out the time that low-concentration sodium hydroxide solution soaks is 10～15 minutes.
9, by claim 1 is described soda cellulose is carried out the vacuum sulfonation, its vacuum tightness is 700mmHg/cm
2More than, the consumption of dithiocarbonic anhydride is 30～60% of a pulp consumption.
10, the concentration of sodium hydroxide solution by the described molten Jie's sodium cellulose xanghate of claim 1 is 1～5%.
11, the concentration of sodium hydroxide solution by claim 1,10 described molten Jie's sodium cellulose xanghates is 2～4%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105466 CN1034938A (en) | 1988-01-27 | 1988-01-27 | The preparation of expansion cellulose sponge |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105466 CN1034938A (en) | 1988-01-27 | 1988-01-27 | The preparation of expansion cellulose sponge |
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| Publication Number | Publication Date |
|---|---|
| CN1034938A true CN1034938A (en) | 1989-08-23 |
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| CN 88105466 Pending CN1034938A (en) | 1988-01-27 | 1988-01-27 | The preparation of expansion cellulose sponge |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927081A (en) * | 2015-06-11 | 2015-09-23 | 宁波尼可海绵科技有限公司 | Foaming device and foaming method for degradable cellulose sponge product |
| CN105237796A (en) * | 2015-10-30 | 2016-01-13 | 江苏赛维环保有限公司 | Fiber porous material preparation method |
| CN105473784A (en) * | 2013-08-09 | 2016-04-06 | 福伊特专利有限公司 | Clothing |
| CN107417980A (en) * | 2017-06-23 | 2017-12-01 | 天长市博资清洁科技有限公司 | The preparation method of wood pulp sponge |
| WO2018196040A1 (en) * | 2017-04-27 | 2018-11-01 | 哈尔滨欧替药业有限公司 | Expansion suppository body for vagina and application thereof |
| CN109081900A (en) * | 2018-07-06 | 2018-12-25 | 山东圣泉新材料股份有限公司 | Modified polyalcohol and preparation method, modified polyurethane material and preparation method and application |
| CN109161057A (en) * | 2018-08-03 | 2019-01-08 | 恒天海龙（潍坊）新材料有限责任公司 | A kind of cellulose foam material low cost and efficient production method |
| CN109984517A (en) * | 2019-03-26 | 2019-07-09 | 南通丰盛纺织品有限公司 | A kind of ventilative sponge matress with antibacterial flame-retardant function |
| CN110354819A (en) * | 2019-08-15 | 2019-10-22 | 广州大学 | A kind of plant cellulose absorption sponge, preparation method and its application |
| CN110982107A (en) * | 2019-12-27 | 2020-04-10 | 北京赛欧兰阻燃纤维有限公司 | Flame-retardant, antibacterial and anti-mite regenerated cellulose foam cotton and preparation method thereof |
-
1988
- 1988-01-27 CN CN 88105466 patent/CN1034938A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105473784B (en) * | 2013-08-09 | 2019-01-08 | 福伊特专利有限公司 | Stretching |
| CN105473784A (en) * | 2013-08-09 | 2016-04-06 | 福伊特专利有限公司 | Clothing |
| US9938665B2 (en) | 2013-08-09 | 2018-04-10 | Voith Patent Gmbh | Clothing |
| CN104927081A (en) * | 2015-06-11 | 2015-09-23 | 宁波尼可海绵科技有限公司 | Foaming device and foaming method for degradable cellulose sponge product |
| CN105237796A (en) * | 2015-10-30 | 2016-01-13 | 江苏赛维环保有限公司 | Fiber porous material preparation method |
| WO2018196040A1 (en) * | 2017-04-27 | 2018-11-01 | 哈尔滨欧替药业有限公司 | Expansion suppository body for vagina and application thereof |
| CN107417980B (en) * | 2017-06-23 | 2019-05-17 | 天长市博资清洁科技有限公司 | The preparation method of wood pulp sponge |
| CN107417980A (en) * | 2017-06-23 | 2017-12-01 | 天长市博资清洁科技有限公司 | The preparation method of wood pulp sponge |
| CN109081900A (en) * | 2018-07-06 | 2018-12-25 | 山东圣泉新材料股份有限公司 | Modified polyalcohol and preparation method, modified polyurethane material and preparation method and application |
| CN109081900B (en) * | 2018-07-06 | 2021-01-26 | 山东圣泉新材料股份有限公司 | Modified polyol and preparation method thereof, modified polyurethane material and preparation method and application thereof |
| CN109161057A (en) * | 2018-08-03 | 2019-01-08 | 恒天海龙（潍坊）新材料有限责任公司 | A kind of cellulose foam material low cost and efficient production method |
| CN109984517A (en) * | 2019-03-26 | 2019-07-09 | 南通丰盛纺织品有限公司 | A kind of ventilative sponge matress with antibacterial flame-retardant function |
| CN110354819A (en) * | 2019-08-15 | 2019-10-22 | 广州大学 | A kind of plant cellulose absorption sponge, preparation method and its application |
| CN110354819B (en) * | 2019-08-15 | 2022-05-03 | 广州大学 | Plant cellulose adsorption sponge, preparation method and application thereof |
| CN110982107A (en) * | 2019-12-27 | 2020-04-10 | 北京赛欧兰阻燃纤维有限公司 | Flame-retardant, antibacterial and anti-mite regenerated cellulose foam cotton and preparation method thereof |
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