CN1039419C - Preparing process for super moisture absorbing resin - Google Patents
Preparing process for super moisture absorbing resin Download PDFInfo
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- CN1039419C CN1039419C CN 92104785 CN92104785A CN1039419C CN 1039419 C CN1039419 C CN 1039419C CN 92104785 CN92104785 CN 92104785 CN 92104785 A CN92104785 A CN 92104785A CN 1039419 C CN1039419 C CN 1039419C
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- absorbing resin
- moisture absorbing
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Abstract
The present invention relates to a method for preparing super water absorbing resin, which is characterized in that after acrylic monomers are partially neutralized by alkali, activated kaolin clay is added, and a porous while solid is obtained through rapid polymerization under the action of a thermal initiator. Then, the porous white solid is pulverized into white power. The product can be widely used in the aspects of agriculture, items in daily use, etc.
Description
The present invention relates to a kind of preparation method of super moisture absorbing resin, belong to the super moisture absorbing resin cross linked polyacrylate, directly apply to that coping with agriculture drought is kept a full stand of seedings, aspect such as aerial seeding aerial sowing, vegetable and fruit are fresh-keeping, daily-use chemical industry.
The preparation method of water-absorbing resin is a lot, mainly contains solution polymerization process, suspension polymerization, inverse suspension polymerization method, the poly-method of speed is a mass polymerization etc.Its purpose all is to improve the water-intake rate and the rate of water absorption of water-absorbing resin, but payes attention to not enough to the cost that reduces product.Disclose a kind of preparation method of High hydrophilous resin in CN1041601A, its purpose is to reduce the cost of product, but it adopts redox initiator polymerization in the aqueous solution, long reaction time, water content is big in the reaction system, dry difficulty, thereby preparation cycle is long.At US4677174, a kind of preparation method of water-absorbing resin is disclosed among the US4820773, its purpose mainly is to use at sanitary towel, require the imbibition body after, gel-strength is big, is not suitable for the agricultural seed dressing and uses, and the product cost height.
The objective of the invention is to avoid above-mentioned weak point of the prior art and provide a kind of technology simple, preparation cycle is short, rate of water absorption height, the super moisture absorbing resin that not only is fit to the agricultural seed dressing but also can be used for using in the sanitary product that cost is lower.
The objective of the invention is to realize by following measure.In having the anticorrosion mixing tank of whipping appts, add vinylformic acid 35-50% weight successively by the reaction mixture gross weight, distilled water 15-20% weight, alkali 25-35% weight, linking agent 0.0025-0.01% weight, stir, and to keep material temperature be 50-55 ℃, add organic solvent 5-7% weight again, the mixture of dissolving initiator 0.25-1% weight, add kaolin 3-10% weight at last, stir, putting into antiseized container carries out speed and gathers into the porousness white solid, and to be dried to water content be below 10%, grinds to particle diameter 0.246～0.175mm (60-80 order) to get final product.By above-mentioned technology and proportioning, make full use of heat of polymerization and drive moisture content and organic solvent in the product away, making swelling polymer is the porousness solid.In reaction mixture, add kaolin and can significantly improve rate of water absorption.In best proportioning, press the reaction mixture gross weight, add vinylformic acid 40% weight, distilled water 19.4% weight, alkali 29.595% weight, linking agent 0.005% weight, organic solvent 6% weight, initiator 0.5% weight, kaolin 4.5% weight.
The present invention makes full use of heat of polymerization and drives moisture content and organic solvent in the product away, makes technology simple, with short production cycle, can finish in 3 hours from being dosed into the finished product, but thereby save energy, the raw material availability height, cost is low, and water-intake rate reaches more than 500 times of own wt, and is pollution-free.Being used as anti-drought water-retaining agent in agroforestry, mainly is that seed dressing is stained with root with plantlet of transplant, can significantly increase seedling rate and surviving rate, shows that according to agriculture indoor test crop can be increased production 10-30%.
Of the present invention details are as follows: add vinylformic acid 35-50% weight successively by the reaction mixture gross weight in glass that has whipping appts or stainless steel mixing vessel, distilled water 15-20% weight, alkaline substance such as sodium hydroxide or potassium hydroxide or yellow soda ash is a 25-35% weight, Tai-Ace S 150 or expression alcohol or N, after N '-linking agents such as methylene bis acrylamide are 0.0025-0.01% weight, stir, and keep by water-bath that material temperature is 50-55 ℃ in the mixing tank, adding acetone or 1: 1 acetone methyl alcohol mixed liquor or 1: 1 organic solvents such as acetone ethanol mixed solution again is 5-7% weight, and dissolve 2,2 '-Diisopropyl azodicarboxylate or with the water dissolution 2 of equivalent percentage ratio, 2 '-after initiators such as azo (2-amidine propane) hydrochloride are 0.25-1% weight, join in the reaction mixture material in the mixing tank, the activated pulverizing that adds 3-10% weight at last is the kaolin behind the particle diameter 0.043mm (325 order) again.Stir, putting into antiseized container that internal surface made by materials such as polypropylene or tetrafluoroethylene carries out speed and gathers into the porousness white solid, and by ventilate or vacuum-drying to become water content be below 10%, grind again to particle diameter 0.246-0.175mm (60-80 order) to get final product.In implementation process, by the gross weight of reaction mixture directly add vinylformic acid 40% weight, distilled water 19.4% weight, alkali 29.595% weight, linking agent O.005% weight, organic solvent 6% weight, initiator O.5% weight, kaolin 4.5% weight be that effect is best, product is best.
Quality product of the present invention is tested mainly examination " water-intake rate ", and three indexs of simulation urine, i.e. urine absorbing rate, suction urinated speed and taken out urine power.The mensuration of water-intake rate is to take by weighing the dried water-absorbing resin of a gram, joins in the 1000ml distilled water, stir park half an hour after, via hole diameter is that 0.074mm (200 order) sieve filters, the milliliter number of statistics filtrate.Calculate:
The mensuration of simulation urine, its proportioning is a distilled water 97.09%, urea 1.94%, sodium-chlor 80% is with the sal epsom 0.11% of seven crystal water, calcium chloride 0.06%.Next is to the mensuration of urine absorbing rate.Take by weighing dried water-absorbing resin 0.2 gram, put in the tea bag of making of tNonwovens (40 * 150mm), this bag immersed in the simulation urine that 100ml prepared, and get a blank bag in addition and do parallel laboratory test, take out after 30 minutes and drain the back and measure two bags of weight.
Once more, to inhaling the mensuration of urine speed, take by weighing water-absorbing resin 1.0 grams, join in the 20ml simulation urine, lose flowability and form expansion glue up to water-absorbing resin, urine is all absorbed time of being experienced for inhaling urine speed.At last, to taking out the mensuration of urine power, get 20ml simulation urine and drip to that (55 * 75mm) make the matrix that contains simulation urine on the thin paper, evenly be sprinkled upon on the matrix 1 gram water-absorbing resin, take out resin expansion glue after ten minutes, and weigh, being decided to be the take out urine power of resin to thin paper, the test data of Shi Yan water-intake rate and simulation urine is as follows several times:
| Test number | Kaolin % (weight) | Water-intake rate mL/ gram | Urine absorbing rate mL/ gram | Inhale urine speed second | Taking out urine makes every effort to overcome/restrains |
| 1 | 4.5 | 600 | 51.4 | 7 | 17.4 |
| 2 | 5 | 550 | 57.5 | 7 | 17.3 |
| 3 | 5 | 560 | 56.4 | 8 | 17.8 |
| 4 | 5 | 580 | 64.8 | 8 | 16.8 |
| 5 | 5 | 550 | 55.3 | 7 | 16.0 |
Embodiment 1
In being furnished with the mixing tank of mechanical stirring device, the vinylformic acid that adds 35 grams successively, 15 gram distilled water, the sodium hydroxide of 25 grams behind the 0.0025 gram Tai-Ace S 150, stirs, and keep by water-bath that material temperature is 50 ℃ in the mixing tank, again with 2,2 ' of 5 acetone solutions that restrain, 0.25 gram---add behind the Diisopropyl azodicarboxylate in the reaction mixture material in people's mixing tank, the activated pulverizing that add 3 grams at last are the kaolin behind the particle diameter 0.043mm (325 order).Stir, the container of putting into the internal surface coating tetrafluoroethylene then carries out speed and gathers into the porousness white solid, goes forward side by side to work that to be dried to water content be below 10% to wind, grinds to particle diameter 0.246mm (60 order) again and obtains the finished product.
Embodiment 2
According to the method for embodiment 1, with the vinylformic acid of 50 grams, 20 gram distilled water, the sodium hydroxide of 35 grams, 0.01 gram Tai-Ace S 150, the acetone of 7 grams, 2,2 ' of 1 gram---Diisopropyl azodicarboxylate, the kaolin of 10 grams.
Embodiment 3
According to the method for embodiment 1, get vinylformic acid 40 grams, distilled water 19.4 grams, sodium hydroxide 29.595 grams, Tai-Ace S 150 0.005 gram, acetone 7 grams, 2,2 '-Diisopropyl azodicarboxylate 0.50 gram, kaolin 4.5 grams.
Embodiment 4
According to the method for embodiment 1 and the batching of embodiment 1,2,3, getting raw material is vinylformic acid, distilled water, and sodium hydroxide, expression alcohol, 1: 1 acetone methyl alcohol mixed liquor, 2,2 '-azo (2-narrows basic propane) the hydrochloride aqueous solution, kaolin.
Embodiment 5
Getting raw material according to the batching of the method for embodiment 1 and embodiment 1,2,3 is vinylformic acid, distilled water, and yellow soda ash, N, N '-methylene bis acrylamide, 1: 1 acetone ethanol mixed solution, 2,2 '-Diisopropyl azodicarboxylate, kaolin.
Embodiment 6
According to the method for embodiment 1 and the proportioning raw materials of embodiment 1,2,3, and the raw material of getting of embodiment 3,4,5, it keeps temperature of charge is 55 ℃, and is that polyacrylic container middling speed is poly-at internal surface, grinds to particle diameter 0.175mm (80 order) by vacuum-drying to get final product.
Claims (8)
1. the preparation method of a super moisture absorbing resin, it is characterized in that the gross weight by reaction mixture adds vinylformic acid 35-50% weight, distilled water 15-20% weight, alkali 25-35% weight, linking agent 0.0025-0.01% weight successively in mixing tank, stir, and to keep material temperature be 50-55 ℃, the mixture that adds organic solvent 5-7% weight, dissolving initiator 0.25-1% weight again, add kaolin 3-10% weight at last, stir, put into container and carry out speed and gather into the porousness white solid, dry, grind.
2. the preparation method of super moisture absorbing resin as claimed in claim 1, the best proportioning that it is characterized in that raw material is: press the gross weight of reaction mixture, vinylformic acid 40% weight, distilled water 19.4% weight, alkali 29.595% weight, linking agent 0.005% weight, organic solvent 6% weight, initiator 0.5% weight, kaolin 4.5% weight.
3. the preparation method of super moisture absorbing resin as claimed in claim 1 is characterized in that alkali is sodium hydroxide, potassium hydroxide, yellow soda ash.
4. the preparation method of super moisture absorbing resin as claimed in claim 1 is characterized in that linking agent is Tai-Ace S 150, expression alcohol, N, N '-methylene bis acrylamide.
5. the preparation method of super moisture absorbing resin as claimed in claim 1 is characterized in that organic solvent is acetone, 1: 1 acetone methyl alcohol mixed liquor, 1: 1 acetone ethanol mixed solution.
6. the preparation method of super moisture absorbing resin as claimed in claim 1, it is characterized in that initiator be 2,2 '-Diisopropyl azodicarboxylate, 2,2 '-azo (2-amidine propane) hydrochloride.
7. the preparation method of super moisture absorbing resin as claimed in claim 1 is characterized in that kaolin is that activated pulverizing back adds 3-10% weight.
8. the preparation method of super moisture absorbing resin as claimed in claim 1, it is characterized in that described mixing tank is the anticorrosion container that has whipping appts, and to keep material temperature by water-bath be 50-55 ℃, in antiseized container, carry out speed at last and gather into the porousness white solid, being dried to water content is below 10%, grinds to particle diameter 0.246～0.175mm (60-80 order) to get final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92104785 CN1039419C (en) | 1992-06-20 | 1992-06-20 | Preparing process for super moisture absorbing resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92104785 CN1039419C (en) | 1992-06-20 | 1992-06-20 | Preparing process for super moisture absorbing resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1080642A CN1080642A (en) | 1994-01-12 |
| CN1039419C true CN1039419C (en) | 1998-08-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92104785 Expired - Fee Related CN1039419C (en) | 1992-06-20 | 1992-06-20 | Preparing process for super moisture absorbing resin |
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| CN (1) | CN1039419C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ZA200106245B (en) * | 2000-08-03 | 2002-02-08 | Nippon Catalytic Chem Ind | Water-absorbent resin, hydropolymer, process for producing them, and uses of them. |
| CN100358926C (en) * | 2005-11-24 | 2008-01-02 | 陕西科技大学 | Process for preparing environment protection type water retaining agent |
| KR20140095569A (en) * | 2006-02-28 | 2014-08-01 | 에보니크 데구사 게엠베하 | Biodegradable superabsorbent polymer composition with good absorption and retention properties |
| CN102702405B (en) * | 2012-07-05 | 2014-04-09 | 东营市诺尔化工有限责任公司 | Method for preparing ultralow-residue water absorbing resins |
| CN104082093A (en) * | 2014-06-16 | 2014-10-08 | 郎溪县双明生态农业有限公司 | Lagerstroemia transplanting method |
| CN111955355A (en) * | 2020-08-05 | 2020-11-20 | 中国农业大学 | Simulated sheep urine and preparation method and application thereof |
| CN116283027B (en) * | 2023-02-03 | 2024-05-10 | 北京市政建设集团有限责任公司 | Engineering soil water reducing agent with high water content, preparation method and application thereof |
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1992
- 1992-06-20 CN CN 92104785 patent/CN1039419C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1080642A (en) | 1994-01-12 |
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