CN1087353A - Acrylate water-absorbing resin manufacture method and equipment - Google Patents
Acrylate water-absorbing resin manufacture method and equipment Download PDFInfo
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- CN1087353A CN1087353A CN 93118705 CN93118705A CN1087353A CN 1087353 A CN1087353 A CN 1087353A CN 93118705 CN93118705 CN 93118705 CN 93118705 A CN93118705 A CN 93118705A CN 1087353 A CN1087353 A CN 1087353A
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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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Abstract
Acrylate water-absorbing resin manufacture method and equipment, its technology characteristics are the pre-treatment under the circulation heating of normal pressure constant-temperature hot water, and vinylformic acid is 1: 2～4.5 with the ratio of solvent, T=38～48 ℃, t=20～30 minute.Pretreated material is divided in the canister, and in T=55～85 ℃, t=0.5～8 hour are with normal pressure constant-temperature hot water circulation heated polymerizable.Gelinite after the polymerization enters vacuum drying oven, and is at P=-0.092～0.098MPa, dry under ℃ condition of T=50～62.Its apparatus characteristic is normal pressure constant-temperature hot water hydronics and vacuum drying system.Gelinite of the present invention is easy to take out from reactor, and save energy reduces degree of oxidation, is easy to suitability for industrialized production.
Description
Acrylate water-absorbing resin manufacture method and equipment belong to the production technique and the production unit technical field of 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.The gelinite that this way forms is difficult to take out from reactor, also just can not form suitability for industrialized production.And existing drying process employing atmospheric steam heat drying method, electric heating wind convective heating desiccating method, these ways power consumptions are big, and rate of drying is slow, the easy oxidation of gelinite.Add in copolymerization and to pine for heat and do not recycle, waste 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 the hot water circulation heating process.Save energy; Drying to gelinite adopts the vacuum-drying heating, makes rate of drying fast, and it is low to consume energy, and 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 ℃ condition of P=-0.092～0.098MPa, T=42～57, 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, is 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=-0.092～0.098MPa, 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, 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 4, extraction hood 9.Housing 5 is for having the bilayer structure of insulation interlayer, upper spacer be located at polymerization canister 38 above, extraction hood be fixed on housing 5 above.Internal heating pipe 6 be located at the polymerization canister below.Upper spacer, polymerization canister, internal heating pipe all are located in the housing.Polymerization canister 38 has and covers 31.
Two of the technical characterictic of production unit is the vacuum drying system of gelinite.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 plate 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 saves the mass production water.Vacuum drying method is than atmospheric steam heat drying method.Electric heating wind convective heating desiccating method has improved rate of drying 30～40%, has reduced the chance of multipolymer and atmospheric oxidation, has improved quality product.The suction multiple is up to 1000 times, and absorption speed is fast, and suction-bleed-drying-suction can be returned multiple carrying out.
Fig. 1 is the schema of production technique of the present invention.
Fig. 2 is the structural representation of heating system.
Fig. 3 is the structural representation of heating tank.
Fig. 4 is the structural representation of vacuum drying system.
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, and places to scribble the dish of not being stained with agent, enters vacuum drying oven, ℃ adopts normal pressure constant-temperature hot water circulation heating 19 hours down 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.This system is made up of heat exchanger 1, recycle pump 2, heating tank 3, 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 by the road, and the hot water after the heat exchanger 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 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 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 intravital 37 on the shell, and is in the top of internal heating pipe and the below of upper spacer, and the polymerization canister has and covers 31.Hot water inlet 25 is on the right side of housing.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 tube.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=-0.092～0.098MPa 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 (6)
1, acrylate water-absorbing resin manufacture method belongs to the production technique of fine chemical product.It includes vinylformic acid and places the rectifying of vacuum still, it is characterized in that 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, cooling and stirring is to neutralization under ℃ condition of T=20～28, 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 is filled with nitrogen, and scribble in the small-sized polymerization tank of separant, capping is placed on carries out polymerization in the heating tank, and polymerizing condition is, the heating of normal pressure constant-temperature hot water, T=55～85 ℃, t=0.5～8 hour.
2, the production unit of acrylate water-absorbing resin it include normal pressure constant-temperature hot water hydronics and normal pressure constant-temperature hot water circulating vacuum dehumidification system; The polymerization heating system is made up of heat exchanger (1), recycle pump (2), heating tank (3), respective line; 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, it is characterized in that heating tank (3) is made up of housing (5), internal heating pipe (6), polymerization canister (38), upper spacer (4), extraction hood (9); 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) and form.
3, the production unit of acrylate High hydrophilous resin according to claim 2, the housing (5) that it is characterized in that heating tank (3) is for having the bilayer structure of insulation interlayer, extraction hood be fixed on housing (5) above, internal heating pipe (6) be located at housing (5) below, polymerization canister (38) is located on the shell intravital (37), and being in the top of internal heating pipe (6) and the below of upper spacer (4), the polymerization canister has lid (31).
4, the production unit of acrylate High hydrophilous resin according to claim 2, it is characterized in that the bleeding point (17) of vacuum drying oven (10) is located at the upper end of housing (16), hot water inlet valve (22) communicates with hot-water line (18), hot-water line (18) communicates with each hot-plate (21), 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 above.
5, acrylate water-absorbing resin manufacture method according to claim 1, it is characterized in that gelinite after the polymerization is placed on scribbles in the dish of not being stained with agent, enter vacuum drying oven, under ℃ condition of P=-0.092～0.098MPa, T=50～62, adopt normal pressure constant-temperature hot water heating 18～20 hours, when dried multipolymer water content is lower than 5%, take out.
6,, it is characterized in that not being stained with agent and mix and form by rubber repel 80～90%, stearic acid 2～3%, ore deposit cured 4～8% according to the manufacture method of claim 1,5 described acrylate water-absorbing resins.
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 true CN1087353A (en) | 1994-06-01 |
| CN1047389C CN1047389C (en) | 1999-12-15 |
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| 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) |
Cited By (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 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0713109B2 (en) * | 1985-09-02 | 1995-02-15 | 三菱油化株式会社 | Method for producing beaded self-crosslinking water-absorbing polymer |
| JPH07119262B2 (en) * | 1987-11-06 | 1995-12-20 | ユニ・チャーム株式会社 | Method for producing water-absorbent composite |
| 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
Cited By (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 |
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| Publication number | Publication date |
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| CN1047389C (en) | 1999-12-15 |
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