CN102212211A - Method for preparing cellulose sponge - Google Patents
Method for preparing cellulose sponge Download PDFInfo
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- CN102212211A CN102212211A CN 201110094497 CN201110094497A CN102212211A CN 102212211 A CN102212211 A CN 102212211A CN 201110094497 CN201110094497 CN 201110094497 CN 201110094497 A CN201110094497 A CN 201110094497A CN 102212211 A CN102212211 A CN 102212211A
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Abstract
The invention relates to a method for preparing a cellulose sponge by the steps of activating cellulose wood pulp, reacting with urea to prepare dry cellulose carbamate, dissolving the dry cellulose carbamate in a dilute sodium hydroxide solution at low temperature to form a cellulose carbamate solution, then adding cotton linter, a pore former, color paste and the like to the cellulose carbamate solution for uniformly mixing, ageing at low temperature, putting in boiled water and then cooking to make the cellulose regenerate, forming gaps after the dissolution of the pore former in water, alternatively washing with water and weak acid until neutrality appears, soaking in the water emulsion of a softener, and the like.
Description
Technical field
The present invention relates to a kind of employing cellulose wood pulp, activate through sodium hydroxide, the dry state cellulose carbamate that makes with urea reaction, under cold condition, dissolve in rare sodium hydroxide solution form cellulose carbamate solution after, mix by adding linters, pore former and mill base etc., ageing at low temperatures, put into the boiling water boiling, make cellulose regenerated, the pore former space that stays soluble in water, after water and weak acid alternately wash and is neutrality, prepare the method for cellulose sponge with operations such as softener immersions.
Technical background
Exhaustion day by day along with the petrochemical industry resource, and the more and more stricter control of environmental pollution, exist raw material in short supply, production process has pollutent to produce, the polyurethane sponge production technique that is difficult to shortcomings such as natural degradation after discarded is restricted, and production technique novel and that can solve the cellulose sponge of resource scarcity problem is arisen at the historic moment.At present, the two kinds of production technique that have that compare success: a kind of is that Mierocrystalline cellulose is converted into soda cellulose earlier, again by soda cellulose and CS
2Reaction and after obtaining cellulose sulfonate, it is dissolved in rare NaOH solution forms viscose.Adopt this viscose, by adding the dough that toughener, pore-forming material, softener etc. are made, during the precipitation bath formed via aqueous acid, cellulose sulfonate hydrolysis has wherein generated Mierocrystalline cellulose, pore former is dissolved in the water simultaneously, in product, stay hole, thereby obtained having the cellulose sponge product of hole.This process using occurring in nature plant cellulose of extensive existence is a raw material, solved raw material problem in short supply, but and products obtained therefrom discarded after natural degradation, non-secondary pollution, but this method is by the preparation of cellulose cellulose sulfonate, and in the production process of follow-up cellulose sponge goods, owing to can produce a large amount of SO
2, H
2Toxic gases such as S, severe contamination atmospheric environment.Also contain many sulfocompounds in the water that is discharged in addition, polluted the water source.Though factory adopted certain methods to reclaim SO as possible in recent years
2, H
2S gas is handled the water of discharging, but still can not be reached the ideal effect, and because the interpolation of some recovery systems has increased the economical load of enterprise, product price is risen, and competitive capacity descends.So this production technique can be eliminated gradually.
The technology of another kind of preparation cellulose sponge be directly with cellulose dissolution in a kind of suitable solvent, and then the method for producing spongy cellulosics.Adopting N-methyl morpholine oxide dissolving cellulos is maximum method of studying at present.As (US Patent:6007750 such as Firgo, 1999-12-28.) Mierocrystalline cellulose inserted moisturely be lower than in 17% the NMMO aqueous solution, pressurized, heated treats that Mierocrystalline cellulose all dissolves, and decompression steams moisture, after making cellulosic viscous solution, stir adding pore former and fortifying fibre formation homogeneous mixture in viscous solution down, the precipitation bath of forming via water precipitates Mierocrystalline cellulose and separates out from solvent again, and activate pore former and make its pore-forming, obtain spongy cellulosics after the flushing.(US Patent:5792399 such as Meister, 1998-08-11) above-mentioned technology is improved, before cellulosic material joins NMMO and water mixture, utilize cellulase that raw material has been carried out pre-treatment earlier, improved cellulosic dissolution rate like this, shortened dissolution time, strengthened dissolving power simultaneously, reduced dissolution conditions.
As can be seen, this technology is simple, with short production cycle, and the toxicity of solvent for use NMMO is lower, and is very little to the pollution of environment, but it is higher to produce the cost of NMMO at present, and the recovery of NMMO difficulty relatively, so this technology industrialization also need be done more work.
Summary of the invention
The objective of the invention is to, a kind of method for preparing cellulose sponge is provided.This method is to adopt the cellulose wood pulp, through the sodium hydroxide activation, make cellulose carbamate with urea reaction after, under cold condition, it is dissolved in the cellulose carbamate solution that is formed with certain viscosity in rare sodium hydroxide solution.Adopt this solution, by adding the dough that toughener, pore-forming material etc. are made, through the boiling water boiling, cellulose carbamate hydrolysis wherein generates Mierocrystalline cellulose, pore former is dissolved in the water simultaneously, has stayed hole in product, thereby has obtained having the cellulose sponge of hole.Concrete operations follow these steps to carry out:
A, cellulose wood pulp are torn into that the length of side is that small pieces about 1cm are immersed in that massfraction is 15%, consumption is that 15 times of Mierocrystalline cellulose quality, temperature are that stir-activating leached after 2 hours in 25 ℃ the aqueous sodium hydroxide solution;
B, activatory soda cellulose among the step a is washed with water, filters, remove after the free alkali lye, add aqueous solution of urea, band aqua dimethylbenzene, stir and heat up except that after anhydrating, dimethylbenzene boiling temperature back flow reaction 2.5 hours, make the degradation production of soda cellulose and urea fully react the generation cellulose carbamate, filter out product, clean the back oven dry with hot water;
C, linters is cut into rectangular about 1.5cm, and to be immersed in the aqueous sodium hydroxide solution degreasing softening;
D, with the cellulose carbamate of dry state among the step b, under cold condition, dissolve in the aqueous sodium hydroxide solution, form the plain carbamate solution of homogeneous fibre;
E, in the steps d cellulose carbamate solution, add the linters among the step c, and pore former and mill base, stirring obtains cellulose sponge and mediates body;
F, cellulose sponge among the step e mediated body and puts into former low temperature maturation 12h after, put into the boiling water boiling, treat that pore former all dissolves the back and takes out, water and weak acid is flushing alternately, drying;
G, with the cavernous body that is shaped among the step f, soak after washing, drying with the water miscible liquid of softener.
Cellulose wood pulp alpha-cellulose content is more than 90% among the step a, and the polymerization degree is 450-750.
Among the step b amount of urea be the Mierocrystalline cellulose quality 2-3 doubly, the dimethylbenzene consumption be the Mierocrystalline cellulose quality 10-20 doubly.
The massfraction that soaks the used aqueous sodium hydroxide solution of linters among the step c is 8-10%.
The polymerization degree of the cellulose carbamate of dry state is 300-550 in the steps d, and nitrogen content is 2.5-4.0%.
The used aqueous sodium hydroxide solution massfraction of dissolving cellulos carbamate is 8-10% in the steps d, temperature is-and 8--3 ℃.
The massfraction of cellulose carbamate solution is 5-7% in the steps d.
The consumption of linters is the 8-35% of dry state cellulose carbamate quality among the step e.
Pore former among the step e is that particle diameter is the sal glauberi particulate mixture that 1-8mm does not wait, and quality is 10-40 a times of dry state cellulose carbamate quality.
The cooking time of the sponge of gelation kneading body is 3-4 hour among the step f.
The main component of softener is fatty alcohol-polyoxyethylene ether (MOA-3) and aliphatic alcohol polyoxyvinethene phosphate (AEP) in the step g.
The massfraction of softener is 3-5% in the step g softener water miscible liquid, and soak time is 5-10 minute.
Of the present invention is a kind of method for preparing cellulose sponge, and this method has:
(1) the reproducible plant cellulose resource of exploitation prepares and Environmental compatibility is good and the cellulose sponge of excellent property.Solved the sponge product that adopts material preparations such as polystyrene, urethane, not only raw material is in short supply, and is difficult to natural degradation, problems such as serious harm existent environment of people after discarded;
(2) the present invention after adopting Mierocrystalline cellulose and urea reaction to prepare cellulose carbamate, is dissolved in the method for preparing cellulose sponge in the sig water with it, has eliminated the waste gas contaminated wastewater from the source.Utilize cellulose sulfonate method production of cellulose sponge technology, exist and produce H in the production process
2S, CS
2Deng obnoxious flavour and contain the pollution problem of S waste water, eliminate or to reduce the equipment input of polluting very big by aftertreatment, thereby product cost is improved, think that therefore the present invention has decontamination, reduces the characteristics of product cost.
Embodiment
Embodiment 1
A, be that sodium hydroxide solution that 450 wood pulp pool tears up back and 150 grams 15% joins in the reaction flasks that 250 persons of outstanding talent rise with the 10 gram polymerization degree, 25 ℃ of following turn on agitator, make Mierocrystalline cellulose and sodium hydroxide solution thorough mixing, stop after 2 hours stirring, leach back water flushing, remove free alkali lye after filter do, insert in the reaction flask, the aqueous solution that adds 20 gram urea, 100 gram dimethylbenzene, turn on agitator also begins to heat up.Treat that moisture has taken off fully, sustained reaction was 2.5 hours after temperature was raised to 137 ℃, stopped heating, equitemperature drops to 70 ℃ to be stopped to stir, and reclaims dimethylbenzene, and the water with same temperature washes product afterwards, oven dry, the 11 gram polymerization degree be 300, nitrogen content is 2.5% dry state cellulose carbamate.
B, take by weighing the above-mentioned cellulose carbamate of 7 grams, stir the massfractions that dissolve in-3 ℃ of 93 grams down and be fully dissolving in 10% the aqueous sodium hydroxide solution, form the plain carbamate solution of homogeneous fibre;
C, take by weighing 0.56 gram linters and be cut into rectangular about 1.5cm to be immersed in massfraction be to leach after softening in 10% aqueous sodium hydroxide solution, add and mix the back in the above-mentioned cellulose carbamate solution thoroughly and add and be placed in the refrigerator ageing after sal glauberi particle that 70 gram particles directly do not wait for 1-8mm and mill base mix 12 hours;
D, will be ageing after 12 hours the kneading body of gelation put into the boiling water boiling 3 hours, make cellulose regeneratedly, pore former all dissolves the back and takes out, after water and weak acid alternately wash and are neutrality, be that the water miscible liquid of 3% softener is soaked after 10 minutes and taken out washing, drying with massfraction.
Embodiment 2
A, be that sodium hydroxide solution that 620 wood pulps is torn up back and 150 grams 15% joins in the reaction flasks that 250 persons of outstanding talent rise with the 10 gram polymerization degree, 25 ℃ of following turn on agitator, make Mierocrystalline cellulose and sodium hydroxide solution thorough mixing, stop after 2 hours stirring, leach, the water flushing, filter is done after removing free alkali lye, inserts in the reaction flask, adds the aqueous solution of 25 gram urea, 150 gram dimethylbenzene, turn on agitator also begins to heat up.Treat that moisture has taken off fully, sustained reaction was 2.5 hours after temperature was raised to 137 ℃, stop heating, equitemperature drops to 70 ℃ to be stopped to stir, reclaim dimethylbenzene, afterwards with the water of same temperature flushing product, oven dry, the 11.4 gram polymerization degree be 480, nitrogen content is 3.47% dry state cellulose carbamate.
B, take by weighing the above-mentioned cellulose carbamate of 6 grams, stir the massfractions that dissolve in-5 ℃ of 94 grams down and be fully dissolving in 9% the sodium hydroxide solution, form the plain carbamate solution of homogeneous fibre;
C, take by weighing 1.2 gram linterss and be cut into rectangular about 1.5cm to be immersed in massfraction be to leach after softening in 9% aqueous sodium hydroxide solution, add and mix the back in the above-mentioned cellulose carbamate solution thoroughly and add and be placed in the refrigerator ageing after sal glauberi particle that 120 gram particles directly do not wait for 1-8mm and mill base mix 12 hours;
D, will be ageing after 12 hours the kneading body of gelation put into the boiling water boiling 3.5 hours, make cellulose regeneratedly, pore former all dissolves the back and takes out, after water and weak acid alternately wash and are neutrality, be that the water miscible liquid of 4% softener is soaked after 7 minutes and taken out washing, drying with massfraction.
Embodiment 3
A, be that sodium hydroxide solution that 750 wood pulps is torn up back and 150 grams 15% joins in the reaction flasks that 250 persons of outstanding talent rise with the 10 gram polymerization degree, 25 ℃ of following turn on agitator, make Mierocrystalline cellulose and sodium hydroxide solution thorough mixing, stop after 2 hours stirring, the water flushing is removed after the filter of free alkali lye does, insert in the reaction flask, the aqueous solution that adds 30 gram urea, 200 gram dimethylbenzene, turn on agitator also begins to heat up.Treat that moisture has taken off fully, temperature is raised to 137 ℃, sustained reaction 2.5 hours, stop heating, equitemperature drops to 70 ℃ to be stopped to stir, and reclaims dimethylbenzene, afterwards with the water of same temperature flushing product, oven dry, the 11.8 gram polymerization degree be 550, nitrogen content is 4% dry state cellulose carbamate.
B, take by weighing the above-mentioned cellulose carbamate of 5 grams, stir the massfractions that dissolve in-8 ℃ of 95 grams down and be fully dissolving in 8% the sodium hydroxide solution, form the plain carbamate solution of homogeneous fibre;
C, take by weighing 1.75 gram linterss and be cut into rectangular about 1.5cm to be immersed in massfraction be to leach after softening in 8% aqueous sodium hydroxide solution, add and mix the back in the above-mentioned cellulose carbamate solution thoroughly and add and be placed in the refrigerator ageing after sal glauberi particle that 200 gram particles directly do not wait for 1-8mm and mill base mix 12 hours;
D, will be ageing after 12 hours the kneading body of gelation put into the boiling water boiling 4 hours, make cellulose regeneratedly, pore former all dissolves the back and takes out, after water and weak acid alternately wash and are neutrality, be that the water miscible liquid of 5% softener is soaked after 5 minutes and taken out washing, drying with massfraction.
Claims (10)
1. the preparation method of a cellulose sponge is characterized in that following these steps to carrying out:
A, cellulose wood pulp are torn into that the length of side is that small pieces about 1cm are immersed in that massfraction is 15%, consumption is that 15 times of Mierocrystalline cellulose quality, temperature are that stir-activating leached after 2 hours in 25 ℃ the aqueous sodium hydroxide solution;
B, activatory soda cellulose among the step a is washed with water, filters, remove after the free alkali lye, add aqueous solution of urea, band aqua dimethylbenzene, stir and heat up except that after anhydrating, dimethylbenzene boiling temperature back flow reaction 2.5 hours, make the degradation production of soda cellulose and urea fully react the generation cellulose carbamate, filter out product, clean the back oven dry with hot water;
C, linters is cut into rectangular about 1.5cm, and to be immersed in the aqueous sodium hydroxide solution degreasing softening;
D, with the cellulose carbamate of dry state among the step b, under cold condition, dissolve in the aqueous sodium hydroxide solution, form the plain carbamate solution of homogeneous fibre;
E, in the steps d cellulose carbamate solution, add the linters among the step c, and pore former and mill base, stirring obtains cellulose sponge and mediates body;
F, cellulose sponge among the step e mediated body and puts into former low temperature maturation 12h after, put into the boiling water boiling, treat that pore former all dissolves the back and takes out, water and weak acid is flushing alternately;
G, with the cavernous body that is shaped among the step f, soak after washing, drying with the water miscible liquid of softener.
2. the described method for preparing cellulose sponge of claim 1 is characterized in that cellulose wood pulp alpha-cellulose content is more than 90% among the step a, and the polymerization degree is 450-750.
3. the described method for preparing cellulose sponge of claim 1, it is characterized in that amount of urea among the step b be the Mierocrystalline cellulose quality 2-3 doubly, the dimethylbenzene consumption be the Mierocrystalline cellulose quality 10-20 doubly.
4. the described method for preparing cellulose sponge of claim 1 is characterized in that the massfraction of the used aqueous sodium hydroxide solution of immersion linters among the step c is 8-10%.
5. the described method for preparing cellulose sponge of claim 1, the polymerization degree that it is characterized in that the cellulose carbamate of dry state in the steps d is 300-550, nitrogen content is 2.5-4.0%.
6. the described method for preparing cellulose sponge of claim 1 is characterized in that the used aqueous sodium hydroxide solution massfraction of dissolving cellulos carbamate is 8-10% in the steps d, temperature is-and 8--3 ℃.
7. the described method for preparing cellulose sponge of claim 1, the massfraction that it is characterized in that cellulose carbamate solution in the steps d is 5-7%.
8. the described method for preparing cellulose sponge of claim 1, the consumption that it is characterized in that linters among the step e is the 8-35% of dry state cellulose carbamate quality, pore former is that particle diameter is the sal glauberi particulate mixture that 1-8mm does not wait, and quality is 10-40 a times of dry state cellulose carbamate quality.
9. the described method for preparing cellulose sponge of claim 1 is characterized in that the cooking time of the sponge kneading body of gelation among the step f is 3-4 hour.
10. the described method for preparing cellulose sponge of claim 1, the main component that it is characterized in that softener in the step g is fatty alcohol-polyoxyethylene ether (MOA-3) and aliphatic alcohol polyoxyvinethene phosphate (AEP), its massfraction in water miscible liquid is 3-5%, and the soak time of cavernous body in the softener water miscible liquid is 5-10 minute.
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Cited By (12)
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|---|---|---|---|---|
| CN102504327A (en) * | 2011-10-22 | 2012-06-20 | 桂林理工大学 | Method for preparing cellulose sponge by utilizing sisal hemp wastes hemp bran and hemp head |
| CN103435848A (en) * | 2013-07-31 | 2013-12-11 | 绍兴中纺院江南分院有限公司 | Preparation method of medical cellulose sponge |
| CN103980368A (en) * | 2014-05-28 | 2014-08-13 | 天津工业大学 | Method for preparing cellulose carbamate through liquid-solid-phase reaction |
| CN104945922A (en) * | 2015-06-11 | 2015-09-30 | 宁波尼可海绵科技有限公司 | Method for producing wood pulp sponge |
| WO2016197931A1 (en) * | 2015-06-11 | 2016-12-15 | 宁波尼可海绵科技有限公司 | Compressed sponge product and manufacturing method therefor |
| 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 |
| CN107501415A (en) * | 2017-08-25 | 2017-12-22 | 孙飞勇 | The preparation method of cellulose carbamate |
| CN107896910A (en) * | 2017-11-30 | 2018-04-13 | 安徽绿雨种业股份有限公司 | A kind of wheat original silkworm egg seedling in greenhouse nursery soil |
| CN107926604A (en) * | 2017-11-30 | 2018-04-20 | 安徽绿雨种业股份有限公司 | A kind of retain water and nutrients wheat original silkworm egg nursery soil |
| 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 |
| CN109880181A (en) * | 2019-03-26 | 2019-06-14 | 宋海军 | A kind of mould proof hydrophobic type sponge and preparation method thereof |
| DE102020113396A1 (en) | 2020-05-18 | 2021-11-18 | Carl Freudenberg Kg | Process for the production of cellulose carbamate molded bodies |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504327A (en) * | 2011-10-22 | 2012-06-20 | 桂林理工大学 | Method for preparing cellulose sponge by utilizing sisal hemp wastes hemp bran and hemp head |
| CN102504327B (en) * | 2011-10-22 | 2013-05-01 | 桂林理工大学 | Method for preparing cellulose sponge by utilizing sisal hemp wastes hemp bran and hemp head |
| CN103435848A (en) * | 2013-07-31 | 2013-12-11 | 绍兴中纺院江南分院有限公司 | Preparation method of medical cellulose sponge |
| CN103980368A (en) * | 2014-05-28 | 2014-08-13 | 天津工业大学 | Method for preparing cellulose carbamate through liquid-solid-phase reaction |
| CN104945922A (en) * | 2015-06-11 | 2015-09-30 | 宁波尼可海绵科技有限公司 | Method for producing wood pulp sponge |
| WO2016197931A1 (en) * | 2015-06-11 | 2016-12-15 | 宁波尼可海绵科技有限公司 | Compressed sponge product and manufacturing method therefor |
| 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 |
| 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 |
| CN107501415A (en) * | 2017-08-25 | 2017-12-22 | 孙飞勇 | The preparation method of cellulose carbamate |
| CN107896910A (en) * | 2017-11-30 | 2018-04-13 | 安徽绿雨种业股份有限公司 | A kind of wheat original silkworm egg seedling in greenhouse nursery soil |
| CN107926604A (en) * | 2017-11-30 | 2018-04-20 | 安徽绿雨种业股份有限公司 | A kind of retain water and nutrients wheat original silkworm egg nursery soil |
| 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 |
| CN109880181A (en) * | 2019-03-26 | 2019-06-14 | 宋海军 | A kind of mould proof hydrophobic type sponge and preparation method thereof |
| DE102020113396A1 (en) | 2020-05-18 | 2021-11-18 | Carl Freudenberg Kg | Process for the production of cellulose carbamate molded bodies |
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Application publication date: 20111012 |