CN1047389C - Method and equipment for preparation of acrylate water-absorbing resin - Google Patents
Method and equipment for preparation of acrylate water-absorbing resin Download PDFInfo
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- CN1047389C CN1047389C CN93118705A CN93118705A CN1047389C CN 1047389 C CN1047389 C CN 1047389C CN 93118705 A CN93118705 A CN 93118705A CN 93118705 A CN93118705 A CN 93118705A CN 1047389 C CN1047389 C CN 1047389C
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
- C08F20/04—Acids, Metal salts or ammonium salts thereof
- C08F20/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract
The present invention relates to a preparation method and equipment for acrylate water absorption resin. The technology of the present invention is characterized in that pretreatment is carried out under the conditions of normal pressure, constant temperature and circular heating of hot water, the ratio of acrylic acid to a solvent is (1 to 2) to 4.5, treatment temperature is from 38 to 48 DEG C, and treatment time is from 20 to 30 minutes; materials are the pretreatment is separately loaded in small tanks and are polymerized under the conditions of normal pressure, constant temperature and circular heating of hot water; gel after polymerization enters a vacuum drying box and is dried under the conditions that pressure is from-0.092 to 0.098MPa, and temperature is from 50 to 62 DEG C. The equipment is characterized in that a hot water circulation heating system of normal pressure and constant temperature and a vacuum drying system are used. The gel is easy to be taken out from a reaction kettle, and the present invention has the advantages of energy saving, oxidation degree reduction and easy industrial production.
Description
The equipment of making vinylformic acid salt solution water-absorbing resin belongs to the production unit technical field of producing fine chemical product.
Having acrylate and vinylformic acid now or forming High hydrophilous resin with the vinyl monomer copolymerization generally all is to adopt a step to concentrate copolymerization process, and the gelinite of this way formation is difficult to take out from reactor, also just can not form suitability for industrialized production.And existing drying process adopts atmospheric steam heat drying method, electric heating wind convective heating desiccating method, and big, slow, the easy oxidation of gelinite of rate of drying of these ways power consumptions adds in copolymerization and to pine for heat and do not recycle, and wastes energy.
The objective of the invention is to design and a kind ofly adopt two step dispersion copolymerization technologies, make the gelinite that forms be easy to from reactor, take out to acrylate and vinylformic acid or with the vinyl monomer copolymerization.In material copolymerization and dry heat process, adopt hot water circulation heating process, save energy.Drying to gelinite adopts the vacuum-drying heating, makes that rate of drying is fast, power consumption is low, reduces degree of oxidation.For realizing that above-mentioned processing step has designed corresponding copolymerization heating installation and gelinite drying plant again.
Manufacturing process of the present invention is for to place the rectifying of vacuum still with commercially available vinylformic acid, rectifying under P=-(0.092～0.098) MPa, T=42～57 ℃ condition, and the vinylformic acid of rectification and purification places the storage tank that is provided with cold and hot system standby.Solvent is placed the reactor that is filled with nitrogen, add vinylformic acid, vinylformic acid is controlled at 1: 2～4.5 with the weight or meausurement ratio of solvent, mixed dissolution under continuous stirring and cooling conditions, treat that fully the dissolving back drips quantitative alkali hydroxide or ammoniacal liquor, temperature is controlled at cooling and stirring under ℃ condition of T=20～28, reaches quantitative neutralization.Add quantitative auxiliary agent then in order, under T=20～36 ℃, fully mix.Be heated to T=38～48 ℃ with normal pressure constant-temperature hot water circulation then, the first step pre-treatment has promptly been finished in t=20～30 minute.Pretreated material is sub-packed in the small-sized polymerization tank.Be filled with nitrogen in the polymerization tank, and scribble and be not stained with agent, capping is placed on carries out polymerization in the heating tank.The circulation heating of normal pressure constant-temperature hot water is still adopted in polymerization, T=55～85 ℃, t=0.5～8 hour.Gelinite water content height after finishing is so also need carry out drying treatment.
Multipolymer takes out jar after rub, place and scribble the special dish of not being stained with agent, enter vacuum drying oven, at P=-(0.092～0.098) MPa, under ℃ condition of T=50～62, adopt normal pressure constant-temperature hot water circulation heating 18～20 hours, when dried multipolymer water content is lower than 5%, take out, through pulverizing, screening, packing.
One of technical characterictic of production unit is polymerization technique normal pressure constant-temperature hot water hydronics.This heating system is made up of heat exchanger 1, recycle pump 2, heating tank 3 and respective line.Its major technique is characterised in that the structure of heating tank 3, and heating tank 3 is made up of heating tank housing 5, internal heating pipe 6, polymerization canister 38, upper spacer 37, lower clapboard 4, extraction hood 9.Housing 5 is for having the bilayer structure of insulation interlayer, upper spacer 37 be located at polymerization canister 38 above, extraction hood 9 be fixed on housing 5 above.Internal heating pipe 6 be located at polymerization canister 38 below.Upper spacer 37, lower clapboard 4, polymerization canister 38, internal heating pipe 6 all are located in the housing 5.Polymerization canister 38 has and covers 31.
Two of the technical characterictic of production unit is the vacuum drying system of gelinite, and dehumidification system is made up of vacuum drying oven 10, heat exchanger 11, buffering storage heat jar 12, current regulator 13, injector 14, water storage tank 15, recycle pump 7,8 and respective line.Its major technique is characterised in that the structure of vacuum drying oven 10.Vacuum drying oven 10 is made up of housing 16, bleeding point 17, hot-water line 18, last hot-plate 19, dish 20, hot-plate 21, hot water inlet valve 22, hot water outlet valve 23.Each dish is all established a hot-plate 21 20 times, and hot-water line 18 all communicates with each hot-plate 21, last hot-plate 19 be in that the superiors coil above.
Vacuum drying method and equipment can be used for the drying of all acrylate series copolymer High hydrophilous resins.Also can be used for starch and acrylonitrile or with the drying of oleic series High hydrophilous resin.The technology of acrylate and vinyl monomer copolymerization is identical with the technology of the above acrylate and acrylic acid copolymer.
Two step dispersion copolymerization methods of the present invention make acrylate and vinylformic acid or are easy to take out from reactor with the gelinite of vinyl monomer copolymerization formation, can realize large-scale industrial production, have improved production efficiency.Adopt hot water circulation heating copolymerization process and equipment, saved the energy, the heat energy utilization rate reaches 60～70%, and saving mass production water, vacuum drying method has improved rate of drying 30～40% than atmospheric steam heat drying method, electric heating wind convective heating desiccating method, reduce the chance of multipolymer and atmospheric oxidation, improved quality product.The suction multiple is up to 1000 times, and absorption speed is fast, and---bleed---drying---suction can be carried out repeatedly in suction.
Fig. 1 is the schema of production technique of the present invention, and Fig. 2 is the structural representation of heating system, and Fig. 3 is the structural representation of heating tank, and Fig. 4 is the structural representation of vacuum drying system, and Fig. 5 is the structural representation of vacuum drying oven.
Embodiment one: commercially available vinylformic acid is placed the rectification under vacuum still, and at vacuum tightness P=-0.095MPa, rectifying under the T=46 ℃ of condition, the rectifying thing places T=16 ℃ acid tank to store standby.Solvent is placed the reactor that is filled with nitrogen, add vinylformic acid, the weight ratio of vinylformic acid and solvent is 1: 4.constantly stir and cooling conditions under mixed dissolution, treat the fully quantitative NaoH of dissolving back dropping, temperature is controlled at that cooling and stirring reaches quantitative neutralization under 26 ℃ of conditions, adds quantitative auxiliary agent then in order, at T=28 ℃ of following restir to thorough mixing.Be heated to T=46 ℃ with the circulation of normal pressure constant-temperature hot water then, t=26 minute, promptly finished the first step pre-treatment.Pretreated material is sub-packed in the small-sized polymerization tank, and the material of every canister splendid attire is not more than 30Kg, is filled with nitrogen in the polymerization tank, and scribbles and be not stained with agent, and capping is placed on carries out polymerization in the heating tank.Normal pressure constant-temperature hot water circulation heating, T=60 ℃, t=6 hour are still adopted in polymerization.
Multipolymer takes out jar after rub, place to scribble the dish of not being stained with agent, enter vacuum drying oven, ℃ following employing normal pressure constant-temperature hot water circulation heating is 19 hours in P=-0.096MPa, T=60 ± 0.2, when reaching 4%, takes out dried multipolymer water content, through pulverizing, sieve, packing.
The agent of not being stained with that present embodiment uses is mixed and is formed by rubber repel 80～90%, stearic acid 2～3%, ore deposit cured 4～8%.
Embodiment two: what one of the production unit of this product was creative is the hot water circulation heating system, and this system is made up of heat exchanger 1, recycle pump 2, heating tank 3 and respective line.The hot water that is come by boiler is divided into two-way through water pipe 26, and one the road 27 enters heat exchanger 1 by the road, and the hot water in the heat exchanger 1 after the cooling 28 returns boiler by the road.Enter the internal heater 6 of heating tank 3 by another road of hot water of water pipe 26 through water pipe 29,30 flow back to boiler by the road then.Hot water by heating tank 3 through hot water outlet 32, recycle pump 2, enter heat exchanger 1, heated hot water is by the road 24, hot water inlet 25 returns heating tank 3.Heating tank 3 is made up of housing 5, internal heating pipe 6, polymerization canister 38, upper spacer 37, lower clapboard 4, extraction hood 9.Housing 5 is for having the bilayer structure of insulation interlayer, extraction hood 9 be fixed on housing 5 above.Upper spacer 37, lower clapboard 4, polymerization canister 38, internal heating pipe 6 all are located in the heating tank housing 5, internal heating pipe 6 be located at shell intravital below.Polymerization canister 38 is located on the intravital upper spacer 37 of shell, and is in the top of internal heating pipe 6 and the below of upper spacer 37, and polymerization canister 38 has and covers 31.Hot water inlet 25 is on the right side of housing, and water outlet 32 is in the left side of housing.
What the production unit of this product was creative two is the vacuum drying system of gelinite.Vacuum drying system is made up of vacuum drying oven 10, heat exchanger 11, buffering storage heat jar 12, current regulator 13, injector 14, water storage tank 15, recycle pump 7,8 and respective line.The hot water that is come by boiler enters heat exchanger 11 through pipeline 33, and the exchange temperature is after pipeline 36 returns boiler.Water in the heat reservoir 12 enters heat exchanger 11 through recycle pump 8, enters loft drier 10 through pipeline 34 again after being heated, and finishes working cycle through hot-plate 21 coolings after pipeline 35 is got back to storage heat jar 12.Water in the water storage tank 15 is got back to water storage tank 15 again after circulation high-pressure pump 7 is squeezed into injector 14, the negative pressure that circulation produces constantly extracts air in the loft drier 10 through current regulator 13.Finally reach negative pressure P=-(0.092～0.098) MPa in the loft drier.Vacuum drying oven 10 is made up of housing 16, bleeding point 17, hot-water line 18, last hot-plate 19, dish 20, hot-plate 21, hot water inlet valve 22, hot water outlet valve 23.Bleeding point 17 is located at the upper end of housing 16, and hot water inlet valve 22 communicates with hot-water line 18, and hot-water line 18 communicates with each hot-plate 21, and hot water outlet valve 23 communicates with opposite side hot-water line 18.All be provided with a dish 20 on each hot-plate 21, last hot-plate 19 be in the superiors dishes above, be used for steam seasoning, so as to not make that dewfall drips.
Claims (3)
1, a kind of equipment of making the acrylate water-absorbing resin is characterized in that the gelinite that it includes behind the after polymerization that is used for that pretreated material carried out the normal pressure constant-temperature hot water circulation heated polymerizable system of after polymerization and is used for rubbing carries out vacuum drying normal pressure constant-temperature hot water circulating vacuum dehumidification system; The heated polymerizable system is made up of heat exchanger (1), recycle pump (2), heating tank (3) and respective line, is used for the pretreated material of packing and carries out the small-sized polymerization tank of polymeric (38) and place in the heating tank (3); Vacuum drying system is made up of vacuum drying oven (10), heat exchanger (11), current regulator (13), buffering storage heat jar (12), injector (14), water storage tank (15), recycle pump (7), (8) and respective line.
2, the equipment of manufacturing acrylate water-absorbing resin according to claim 1 is characterized in that heating tank (3) is made up of housing (5), internal heating pipe (6), small-sized polymerization tank (38), upper spacer (37), lower clapboard (4), extraction hood (9); The housing (5) of heating tank (3) is for having the bilayer structure of insulation interlayer, extraction hood (9) be fixed on housing (5) above, internal heating pipe (6) be located at housing (5) below, small-sized polymerization tank (38) is located under the intravital upper spacer of shell (37), and is in the top of internal heating pipe (6).
3, the equipment of manufacturing acrylate water-absorbing resin according to claim 1, it is characterized in that vacuum drying oven (10) by housing (16), bleeding point (17), hot-water line (18), go up hot-plate (19), dish (20), hot-plate (21), hot water inlet valve (22), hot water outlet valve (23) that the gelinite behind the after polymerization of rubbing is housed form.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93118705A CN1047389C (en) | 1993-10-15 | 1993-10-15 | Method and equipment for preparation of acrylate water-absorbing resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93118705A CN1047389C (en) | 1993-10-15 | 1993-10-15 | Method and equipment for preparation of acrylate water-absorbing resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1087353A CN1087353A (en) | 1994-06-01 |
| CN1047389C true CN1047389C (en) | 1999-12-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93118705A Expired - Fee Related CN1047389C (en) | 1993-10-15 | 1993-10-15 | Method and equipment for preparation of acrylate water-absorbing resin |
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| CN (1) | CN1047389C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322029C (en) * | 2002-06-19 | 2007-06-20 | 杨头雄 | Biological decomposability, water absorbent resin and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6253310A (en) * | 1985-09-02 | 1987-03-09 | Mitsubishi Petrochem Co Ltd | Production of beadlike self-crosslinking water-absorbing polymer |
| JPH01121308A (en) * | 1987-11-06 | 1989-05-15 | Mitsubishi Petrochem Co Ltd | Production of water absorbing complex |
| JPH03115313A (en) * | 1989-09-28 | 1991-05-16 | Kazuo Saotome | Production of water-absorptive resin |
-
1993
- 1993-10-15 CN CN93118705A patent/CN1047389C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6253310A (en) * | 1985-09-02 | 1987-03-09 | Mitsubishi Petrochem Co Ltd | Production of beadlike self-crosslinking water-absorbing polymer |
| JPH01121308A (en) * | 1987-11-06 | 1989-05-15 | Mitsubishi Petrochem Co Ltd | Production of water absorbing complex |
| JPH03115313A (en) * | 1989-09-28 | 1991-05-16 | Kazuo Saotome | Production of water-absorptive resin |
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| Publication number | Publication date |
|---|---|
| CN1087353A (en) | 1994-06-01 |
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