CN1080642A - A kind of preparation method of super moisture absorbing resin - Google Patents
A kind of preparation method of super moisture absorbing resin Download PDFInfo
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- CN1080642A CN1080642A CN 92104785 CN92104785A CN1080642A CN 1080642 A CN1080642 A CN 1080642A CN 92104785 CN92104785 CN 92104785 CN 92104785 A CN92104785 A CN 92104785A CN 1080642 A CN1080642 A CN 1080642A
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- absorbing resin
- moisture absorbing
- super moisture
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Abstract
A kind of preparation method of super moisture absorbing resin is characterized in that the present invention utilizes Acrylic Acid Monomer after alkali partly neutralizes, and adds activation kaolin, through the effect of thermal initiator, carries out speed and gathers and make a kind of porous white solid, becomes white powder after crushed.This product is widely used in aspects such as agricultural and daily living article.
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 in sanitary towel, require the imbibition body after, gel-strength is big, is not suitable for 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%), distilled water (15-20%), alkali (25-35%), linking agent (0.0025-0.01%) successively, stir, and keep material temperature for (50-55 ℃), the mixture that adds organic solvent (5-7%) dissolving initiator (0.25-1%) again, 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 the 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, vinylformic acid 40%, distilled water 19.4%, alkali 29.595%, linking agent 0.005%, organic solvent 6%, initiator 0.5%, 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 that technology is simple, it is short to produce all devices, 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 (35-55%) in glass that has whipping appts or stainless steel mixing vessel successively, distilled water (15-20%), alkaline substance such as sodium hydroxide or potassium hydroxide or yellow soda ash is (25-35%), Tai-Ace S 150 or expression alcohol or N, after N '-linking agents such as methylene bis acrylamide are (0.0025-0.01%), stir, and keep in the mixing tank material temperature by water-bath and be (50-55 ℃), add acetone or 1: 1 acetone methyl alcohol mixed liquor or 1: 1 organic solvents such as acetone ethanol mixed solution again and be (5-7%), and dissolve 2,2 '-azo two isobutyls are fine or with the water dissolution 2 of equivalent percentage ratio, 2 '-initiators such as azo (2-narrows basic propane) hydrochloride are for after (0.25-1%), join in the reaction mixture material in the mixing tank, the activated pulverizing that adds (3-10%) (monomer weight is a benchmark) at last is the kaolin behind 325 orders again.Stir, put into container that internal surface made by materials such as polypropylene or tetrafluoroethylene and carry out speed and gather into the porousness white solid, and by ventilate or vacuum-drying to become water content be below 10%, grind again to (60-80) order to get final product.In experiment, directly add vinylformic acid 40%, distilled water 19.4%, alkali 29.595%, linking agent 0.005%, organic solvent 6%, initiator 0.5%, kaolin 4.5%(weight) best for effect, 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 Ke, joins in the 1000ml distilled water, stir park half an hour after, filter the milliliter number of statistics filtrate through 200 mesh sieves.Calculate:
Water-intake rate=(1000ml-filtrate ml)/(dried resin is heavy)
The mensuration of simulation urine, its proportioning is a distilled water 97.09%, urea 1.94%, sodium-chlor 0.80% 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 test, take out after 30 minutes and drain the back and measure two bags of weight.
Water-intake rate (gram/gram)=(suction back (bag+resin)-blank bag is heavy)/(dried resin is heavy)
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 % | Water-intake rate | Urine absorbing rate | Inhale urine speed | Take out urine power |
| Monomer weight is a benchmark | The ml/ gram | The ml/ gram | Second | Gram/gram | |
| 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, add 35% vinylformic acid successively, 15% distilled water, 25% sodium hydroxide behind 0.0025% Tai-Ace S 150, stirs, and keep by water-bath that material temperature is 50 ℃ in the mixing tank, use again 2,2 of 5% acetone solution 0.25 '-the fine back of azo two isobutyls adds in the reaction mixture material in the mixing tank, adding the 3%(monomer weight at last is benchmark) activated pulverizing be kaolin behind 325 orders.Stir, put into internal surface then and carry out speed by the container of tetrafluoroethylene and gather into the porousness white solid, go forward side by side and work that to be dried to water content be below 10% to wind, grinding is that 60 orders obtain the finished product again.
Embodiment 2
According to the method for embodiment 1, the vinylformic acid with 50%, 20% distilled water, 35% sodium hydroxide, 0.01% Tai-Ace S 150,7% acetone, 1% 2,2 '-kaolin of azo two isobutyls fine 10%.Embodiment 3
Embodiment 3
According to the method for embodiment 1, get vinylformic acid 40%, distilled water 19.4%, sodium hydroxide 29.595%, Tai-Ace S 150 0.005%, acetone 7%, 2,2 '-azo two isobutyls are fine 0.05%, high soil 4.5%.
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 '-azo two isobutyls are fine, kaolin.
Embodiment 6
According to the method for embodiment 1 and the proportioning raw materials of embodiment 1,2,3, and embodiment 3,4,5, the raw material of getting, it keeps temperature of charge is 55 ℃ and is that polyacrylic container middling speed is poly-at internal surface, grinding by vacuum-drying is that 80 orders get final product.
Claims (8)
1, a kind of preparation method of super moisture absorbing resin, it is characterized in that in mixing tank, adding successively vinylformic acid (35-50%), distilled water (15-20%), alkali (25-35%), linking agent (0.0025-0.01%), stir, and keep material temperature for (50-55 ℃), add the mixture of organic solvent (5-7%) dissolving initiator (0.25-1%) 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, as the preparation method of claim 1 described super moisture absorbing resin, it is characterized in that the best proportioning of raw material is: vinylformic acid 40%, distilled water 19.4%, alkali 29.595%, linking agent 0.005%, organic solvent 6%, initiator 0.5%, kaolin 4.5%(weight).
3,, it is characterized in that alkali is sodium hydroxide, potassium hydroxide, yellow soda ash etc. as the preparation method of claim 1 described super moisture absorbing resin.
4,, it is characterized in that linking agent is Tai-Ace S 150, expression alcohol, N, N '-methylene bis acrylamide etc. as the preparation method of claim 1 described super moisture absorbing resin.
5,, it is characterized in that organic solvent is acetone, 1: 1 acetone methyl alcohol mixed liquor as the preparation method of claim 1 described super moisture absorbing resin.1: 1 acetone ethanol mixed solution.
6, as the preparation method of claim 1 described super moisture absorbing resin, it is characterized in that initiator be 2,2 '-azo two isobutyls are fine, 2,2 '-azo (2-narrows basic propane) hydrochloride etc.
7,, it is characterized in that kaolin is that activated pulverizing back adds (3-10%) (monomer weight is a benchmark) as the preparation method of claim 1 described super moisture absorbing resin
8, as the preparation method of claim 1 described super moisture absorbing resin, it is characterized in that described mixing tank is the anticorrosion container that has whipping appts, and keep material temperature for (50-55 ℃) by water-bath, 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 the 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 true CN1080642A (en) | 1994-01-12 |
| CN1039419C 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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| Country | Link |
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| CN (1) | CN1039419C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100358926C (en) * | 2005-11-24 | 2008-01-02 | 陕西科技大学 | Process for preparing environment protection type water retaining agent |
| CN1908020B (en) * | 2000-08-03 | 2011-04-27 | 株式会社日本触媒 | Process for producing water-absorbent resin, and uses thereof |
| CN101074300B (en) * | 2006-02-28 | 2012-10-03 | 赢创施托克豪森有限责任公司 | Good absorption and retention properties biodegradable superalborbent polymer composition |
| CN102702405A (en) * | 2012-07-05 | 2012-10-03 | 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 |
| CN116283027A (en) * | 2023-02-03 | 2023-06-23 | 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 |
-
1992
- 1992-06-20 CN CN 92104785 patent/CN1039419C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1908020B (en) * | 2000-08-03 | 2011-04-27 | 株式会社日本触媒 | Process for producing water-absorbent resin, and uses thereof |
| CN100358926C (en) * | 2005-11-24 | 2008-01-02 | 陕西科技大学 | Process for preparing environment protection type water retaining agent |
| CN101074300B (en) * | 2006-02-28 | 2012-10-03 | 赢创施托克豪森有限责任公司 | Good absorption and retention properties biodegradable superalborbent polymer composition |
| CN102702405A (en) * | 2012-07-05 | 2012-10-03 | 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 |
| CN116283027A (en) * | 2023-02-03 | 2023-06-23 | 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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| Publication number | Publication date |
|---|---|
| CN1039419C (en) | 1998-08-05 |
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