CN1546540A - Method and device for preparing water-absorbent resin - Google Patents
Method and device for preparing water-absorbent resin Download PDFInfo
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- CN1546540A CN1546540A CNA2003101115894A CN200310111589A CN1546540A CN 1546540 A CN1546540 A CN 1546540A CN A2003101115894 A CNA2003101115894 A CN A2003101115894A CN 200310111589 A CN200310111589 A CN 200310111589A CN 1546540 A CN1546540 A CN 1546540A
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- internal recycle
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Abstract
The invention discloses a process for preparing absorbent resin comprising, charging water, sodium hydroxide, acrylic acid, N, N'-methylene di-propenamide and potassium peroxodisulfate into stirring still, homogenizing, going through preheating section, reaction section, heat preservation section in sequence, carrying out heat exchange and polymerization reaction.
Description
Technical field
The present invention relates to a kind of preparation method of water-absorbing resin, the invention still further relates to a kind of Continuous Flow waterline reaction unit that integrates static polymerization, heat exchange, section moulding function, be applicable to sanitary towel, disposable diaper, industrial water-retaining agent and farming, forestry and gardening water-holding agent, dewatering agent etc.
Background technology
Up to the present, the production method of patent report water-absorbing resin has had multiple.For example, Japanese Patent discloses clear 56 (1981)-181.408, clear 57 (1982)-94.011, clear 57 (1982)-158.209, clear 57 (1982)-198.714 and Chinese patent 98119318, and their adopt inverse suspension polymerization principle.
Take inverse suspension polymerization method, need a large amount of organic solvents, therefore, the shortcoming of this method is tangible.At first, organic solvent not only causes the influence to Working environment and ecotope, and can bring danger such as contingent burning, blast in using and storing.In order to prevent the leakage of organic solvent, production equipment more complicated, cost are also than higher.Recovery of Organic Solvent further makes the inverse suspension polymerization method equipment configuration quite expensive.Simultaneously, the price of organic solvent itself and inevitably consumption cause the required operational cost of inverse suspension polymerization method to increase.In addition, because in the product of inverse suspension polymerization, some is residual in organic solvent federation, although be micro-, also must manage to remove from product, has increased the complicacy of production process.
Adopt the method for aqueous solution polymerization principle to avoid above-mentioned shortcoming.Japanese Patent discloses clear 57 (1982)-34.101, clear 48 (1973)-42.466, clear 58 (1983)-49.714, clear 50 (1984)-37.003, U.S. Pat-4.286.082, US-4.625.001, US-4.654.039, and Chinese patent 90105865 have disclosed aqueous solution polymerization method.The generative process of the cross-linked polymer of this method relates generally to water-soluble monomer and carries out the radical aqueous solution polymerization and change aquogel polymer in the water of cheapness.
For realizing carrying out effectively the radical aqueous solution polymerization, particularly overcome the reaction later stage, because the raising of the polymerization degree, the viscosity of whole system is high, bring very big difficulty to stirring, U.S. Pat-4.625.001 has disclosed in the reactor of paddle wheel is housed and has matched with polymerization starter, and comes the disperse water gelatin polymer by the shearing force that paddle wheel produced in polymerization process thereupon.According to these patents, in the reactor that generates aquogel polymer, it is indispensable requirement that special polynary rotation paddle wheel is housed.The exemplary that satisfies the equipment of this requirement includes double arm kneading mixer and three arm kneaders, rotation stir shaft in the kneader is with opposite direction with identical or different speed rotation, when two rotation stir shafts rotate with identical speed, the state of used kneader is that two rotation radius of rotating stir shaft overlap part, when the speed of rotating not simultaneously, the state of used kneader is that above-mentioned radius will be avoided overlapping: rotating stir shaft can be σ type, δ type, S type, closed type, fish tail type etc.But, even in these methods, have these characteristics, produce have high-hydroscopicity can water-absorbing resin remain the difficulty.Reason is the measure that attempt comes the disperse water gelatin polymer by the shearing force that paddle wheel produced, and these shearing forces produce simultaneously to generating the disadvantageous effect of High hydrophilous resin polyreaction.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of High hydrophilous resin.Present method is come oxygen in the secluding air effectively by the static and maintenance system vapour pressure in reaction system interface, thereby need not take above-mentioned patent to import the special measure of rare gas elementes such as nitrogen, more avoid mechanical stirring generating the detrimentally affect of the enough big polymkeric substance of molecular weight.The inventive method is simple and direct, and is easy to operate.
A purpose in addition of the present invention provides a kind of Continuous Flow production line apparatus for preparing water-absorbing resin, it integrates static polymerization, heat exchange, section moulding function, reduce facility investment significantly, production process safety, stablize, control easily, be convenient to realize automatization, and made full use of reaction heat, further saved process cost, reduced production cost.
To achieve these goals, the present invention takes following measure:
By control reacting material concentration and temperature of reaction, guarantee to realize static polymerization.Specific practice is: it is 20 to 50% moles that the hierarchy of control contains acid function base monomer (as vinylformic acid, acrylamide etc.) concentration, and 30 to 90% moles monomer is neutralized by alkali.Temperature of reaction system is stabilized in 50-70 ℃ of scope, and the vapour pressure of system is the oxygen in the secluding air effectively, carries out polyreaction.
Adopt the Continuous Flow production line apparatus to realize the heat exchange and the controlled polymerization temperature of reaction of whole reaction system.This device is made up of system's groove 9, transmission belt 8, heat-transfer medium 7 and reactor A a plurality of (illustrating with 22 little square frames among Fig. 1).These reactor A are contained on the transmission belt 8, in the reactor A imbedding system groove 9, heat-transfer medium 7 are arranged in system's groove 9.
Each reactor A is made up of reaction vessel 1, reactor cap 2, internal recycle cooler inlet pipe 3, internal recycle water cooler 4, internal recycle cooler outlet pipe 5 and built-in template 6.A reactor cap 2 is arranged above the reaction vessel 1, be provided with built-in template 6, internal recycle cooler inlet pipe 3, internal recycle water cooler 4, internal recycle cooler outlet pipe 5 in the reaction vessel 1, they are fixed on the reactor cap 2.
According to the polymerisation run of material in the reactor, the Continuous Flow waterline spatially can further be divided into feed location 11, preheating section 12, conversion zone 13, holding-zone 14 and discharging position 15 as shown in Figure 1.
In the Continuous Flow production line apparatus system groove 9, a plurality of reactor A are set, one side has been disperseed material, has been easy to solve the heat dissipation problem of each reactor, can make full use of the reaction heat that the reactor that enters conversion zone is emitted on the other hand, come preheating to be in preheating section reactor internal reaction thing and keep the reactor temperature that is in holding-zone, realize heat exchange in internal system, saved the energy.Simultaneously, owing to take the Continuous Flow production line apparatus, solved the auxiliary shortcoming that the cycle is long, throughput is low, labour intensity is big of general batch reactor production.
Internal recycle cooler inlet pipe 3, internal recycle water cooler 4, internal recycle cooler outlet pipe 5 are set in reactor A, solve general mechanical stirring and reacting kettle jacketing heat exchange and be difficult to the timely difficult problem that a large amount of reaction heat of high viscosity polymerization reaction system are shifted out rapidly, realized effective control to temperature of reaction, prevent temperature runaway and implode, guarantee the security and the quality product of process.
In reactor A, be provided with built-in template 6, made up the real-time forming technique of hydrogel, solve further that polymerization product is attached on the reactor, the discharging difficulty, and need be provided with in addition that specific equipments such as resin slicer machine are cut into slices, the problem of moulding.The material that reaction vessel of the present invention adopts and products with adhesive power is little is made, and material has acid-resistant corrosion, and container shapes is a flat configuration, has both helped the reaction heat radiation, also makes product be easy to discharging from reaction vessel.After the polyreaction, polymkeric substance can be deviate from reactor easily, and extrusion rate reaches 99.9%.
Owing to be on the basis of internal recycle cooling reactor, to carry out this technical combinations, there is not big difficulty in the device fabrication.The a small amount of manufacturing expense that is increased, investment and process cost compared with the slicing machine of saving etc. are actually small.
The present invention compared with prior art, have the following advantages and effect: the present invention proposes the method that a kind of Continuous Flow waterline reaction unit that integrates static polymerization, heat exchange, section moulding function prepares water-absorbing resin, has overcome this area conventional art equipment therefor complexity, temperature control difficulty, problem that process cost is high effectively.Reduced significantly that investment, preparation process are simple and direct, stable, easy handling, saved the energy, reduced productive expense.
Description of drawings
Fig. 1 is a kind of Continuous Flow production line apparatus structural representation;
Fig. 2 is a kind of synoptic diagram of internal recycle cooling reactor of built-in template.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail:
The preparation process of a kind of suction, water-retaining resin is:
A, successively with 5830 parts of water, 950 parts of sodium hydroxide, 2053 parts of vinylformic acid, 1 part of N, N '-methylene-bisacrylamide and 1.2 parts of Potassium Persulphates add common lass lining stirring tank, stir evenly;
B, above-mentioned raw materials is added in the reaction vessel 1;
C, reaction vessel 1 should be in the charging position place of flow-line equipment;
D, reaction raw materials is housed reactor A under the effect of assembly line conveying device 8, leave charging position 11, by counterclockwise, in apparatus system groove 9, by preheating section 12, conversion zone 13, holding-zone 14, temperature is 50-70 ℃, reaches discharging position 15 at last successively.Heat exchange medium 7 in the flow-line equipment system groove 9 plays a role, in time shift out the unnecessary heat of reactor A of conversion zone 13, heating or insulation for material in the reactor A that is in preheating section 12 and holding-zone 14, made full use of the heat that polyreaction is sent, guaranteed that the reaction mass temperature of conversion zone 13 can be too not high.
E, import heat exchange mediums 7 by internal recycle cooler inlet pipe 3, enter the internal recycle water cooler 4 of appendix in reactor cap 2, material in the reaction vessel 1 is carried out heat exchange, heat exchange medium 7 leaves container from internal recycle cooler outlet pipe 5 again, guarantee that the whole reaction system temperature-stable at 50-70 ℃, carries out polyreaction.
F, reactor A after arriving discharging position 15 along with streamline transmits are opened reactor cap 2, take out built-in template 6.Before this, product under the effect of template, is finished excision forming, obtains the polymerization product of definite shape.By difform template, can obtain the gel state product of bulk, strip, sheet etc. respectively.Take out in type gel product at last.
This gel state product, drying is ground into powder to water content＜8%.The water absorbent rate of measuring the gained water-absorbing resin reaches 611-653g/g.
The measuring method of water absorbent rate is: taking by weighing quality is W
1(g) dry resin soaked in tap water after 24 hours, took out the jello that resin suction back forms with screen cloth, and the water of drench attachment removal claims that the jello quality is W
2(g).Q=(W by formula
2-W
1)/W
1, calculate the water absorbent rate Q of this resin.
Claims (3)
1, a kind of preparation method of water-absorbing resin comprises the following steps:
A, successively with water, sodium hydroxide, vinylformic acid, N, N '-methylene-bisacrylamide and Potassium Persulphate add common lass lining stirring tank, stir evenly;
B, above-mentioned raw materials is added in the reaction vessel (1);
C, reaction vessel (1) are in the charging position place of flow-line equipment;
D, the reactor (A) of reaction raw materials is housed under the effect of assembly line conveying device (8), leave charging position (11), by counterclockwise, in apparatus system groove (9), by preheating section (12), conversion zone (13), holding-zone (14), reach discharging position (15) at last successively;
E, import heat exchange medium (7) by internal recycle cooler inlet pipe (3), enter the internal recycle water cooler (4) of appendix in reactor cap (2), the interior material of reaction vessel (1) is carried out heat exchange, heat exchange medium (7) leaves container from internal recycle cooler outlet pipe (5) again, carries out polyreaction;
F, reactor (A) after arriving discharging position (15) along with streamline transmits are opened reactor cap (2), take out built-in template (6).
2, the preparation method of a kind of water-absorbing resin according to claim 1 is characterized in that preheating section (12), conversion zone (13), holding-zone (14) temperature are controlled at 50-70 ℃.
3, a kind of device that is used to realize the method for claim 1, this device comprises:
A kind of reactor (A), system's groove (9), transmission belt (8), heat-transfer medium (7);
Reactor (A) is made up of reaction vessel (1), reactor cap (2), internal recycle cooler inlet pipe (3), internal recycle water cooler (4), internal recycle cooler outlet pipe (5) and built-in template (6);
Reactor (A) is contained on the transmission belt (8), in reactor (A) the imbedding system groove (9), heat-transfer medium (7) is arranged in system's groove (9);
The top reactor cap of reaction vessel (1) (2) is provided with built-in template (6), internal recycle cooler inlet pipe (3), internal recycle water cooler (4), internal recycle cooler outlet pipe (5) in the reaction vessel (1), be fixed on the reactor cap (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111589 CN1235926C (en) | 2003-12-16 | 2003-12-16 | Method and device for preparing water-absorbent resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111589 CN1235926C (en) | 2003-12-16 | 2003-12-16 | Method and device for preparing water-absorbent resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1546540A true CN1546540A (en) | 2004-11-17 |
| CN1235926C CN1235926C (en) | 2006-01-11 |
Family
ID=34336205
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200310111589 Expired - Fee Related CN1235926C (en) | 2003-12-16 | 2003-12-16 | Method and device for preparing water-absorbent resin |
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| Country | Link |
|---|---|
| CN (1) | CN1235926C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992427A (en) * | 2014-06-05 | 2014-08-20 | 长春理工大学 | Oil shale dry distillation slag-acrylic water-absorbent resin in-situ polymerization method |
| CN109081887A (en) * | 2018-08-10 | 2018-12-25 | 安徽富瑞雪化工科技股份有限公司 | A kind of super absorbent resin |
-
2003
- 2003-12-16 CN CN 200310111589 patent/CN1235926C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992427A (en) * | 2014-06-05 | 2014-08-20 | 长春理工大学 | Oil shale dry distillation slag-acrylic water-absorbent resin in-situ polymerization method |
| CN109081887A (en) * | 2018-08-10 | 2018-12-25 | 安徽富瑞雪化工科技股份有限公司 | A kind of super absorbent resin |
| CN109081887B (en) * | 2018-08-10 | 2021-06-29 | 安徽富瑞雪化工科技股份有限公司 | High water absorption resin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1235926C (en) | 2006-01-11 |
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