CN114316107B - Novel production method of super absorbent resin - Google Patents
Novel production method of super absorbent resin Download PDFInfo
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- CN114316107B CN114316107B CN202210015994.9A CN202210015994A CN114316107B CN 114316107 B CN114316107 B CN 114316107B CN 202210015994 A CN202210015994 A CN 202210015994A CN 114316107 B CN114316107 B CN 114316107B
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Abstract
The invention provides a novel production method of a super absorbent resin, which comprises the following steps: adding acrylic acid into a reaction kettle, and then dropwise adding sodium hydroxide for neutralization; sequentially adding an initiator A, an initiator B and a water absorption accelerator C into a reaction kettle, and adding an extruder at 70-90 ℃ for polymerization reaction for 1-5 min after materials are uniformly mixed; extruding the polymerized sizing material into a linear shape through a head opening die of an extruder, and cutting into colloidal particles at a granulator at the head; in the process of granulating, spraying an anti-sticking agent outside the surface of the colloidal particle; and drying and crushing the particles after cutting. The invention has the advantages that: (1) In the polymerization reaction, an initiator A, an initiator B and a water absorption accelerator C are added, so that the reaction is more sufficient, and the reaction time is greatly shortened; (2) Extruding the gelatinous substance after the polymerization reaction into linear adhesive tapes, and greatly reducing the time consumption in the subsequent granulating operation; (3) In the granulating process, an anti-sticking agent is sprayed outside the surface of the colloidal particles, so that the adhesion of the colloidal particles is effectively prevented.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a novel production method of a high water absorption resin.
Background
The super absorbent resin is a novel synthetic polymer material capable of absorbing 500-1000 times of water, has high water absorption performance of absorbing hundreds to thousands of times of liquid than the self weight, and can swell immediately after being swelled into hydrogel when being absorbed by water, so that the liquid is kept in a non-flowing state, and the liquid is difficult to separate even though the pressure is applied. Therefore, the super absorbent resin has wide application in various fields of sanitary articles, industrial and agricultural production, civil construction and the like, and particularly has very wide application in the aspect of preparing paper diapers.
At present, the production method of the super absorbent resin comprises the following steps: firstly, carrying out neutralization reaction on acrylic acid and sodium hydroxide, adding an initiator and the like for mixing after the neutralization reaction, and carrying out high-temperature polymerization on the mixture in a drying tunnel with the length of 150 meters on a driving belt to obtain a rubber block; extruding the gel block through an extruder to form particles after high-temperature polymerization; and (3) after granulating, drying and fine powder to finally obtain the super absorbent resin powder required by the target. The method mainly has the following problems: (1) The high-temperature polymerization reaction time is at least 1.5h, and the production efficiency of the high-hydroscopicity resin is greatly influenced due to the overlong time; (2) The gelatinous substance after the high-temperature polymerization reaction is a gelatinous block, and the time consumption is longer in the subsequent granulating process; (3) In the extrusion and granulating process, colloidal particles are easy to adhere, and the following fine crushing process is affected.
Accordingly, there is an urgent need to design a novel production method of the super absorbent resin.
Disclosure of Invention
The invention aims to solve the technical problems of providing a novel production method of a high-hydroscopicity resin which has short high-temperature polymerization reaction time, high extrusion and granulating efficiency and difficult adhesion of granulated colloidal particles.
The invention adopts the following technical scheme to solve the technical problems:
a novel production method of a super absorbent resin comprises the following steps:
(1) Firstly, adding acrylic acid into a reaction kettle, and then, dropwise adding sodium hydroxide for neutralization; the reaction temperature of the neutralization reaction is 20-45 ℃ and the reaction time is 1.5-3 h;
(2) Adding an initiator A into a reaction kettle after the neutralization reaction, adding an initiator B after the mixing, and finally adding a water absorption accelerator C for mixing; the temperature of the reaction kettle is controlled to be not more than 40 ℃ in the mixing process;
(3) After the materials in the step (2) are fully and uniformly mixed, adding the mixture into an extruder which is kept at a constant temperature of 70-90 ℃ for polymerization reaction for 1-5 min;
(4) An orifice plate type die head is arranged at the outlet of the machine head of the extruder; extruding the polymerized sizing material into a linear shape through a head opening die of an extruder, and cutting into colloidal particles at a granulator at the head; wherein, during the grain cutting process, anti-sticking agent is sprayed outside the surface of the colloidal particle to prevent the colloidal particle from adhesion;
(5) Drying the cut particles at 140-170 ℃, and then finely crushing the particles into the target super absorbent resin product.
In a preferred embodiment of the present invention, in the step (1), the total amount of sodium hydroxide added is 70 to 85% of acrylic acid, and the neutralization degree is controlled to be 70 to 85%.
In the step (2), the initiator a is a peroxide, the initiator B is a reducing substance, and the water absorption enhancer C is a surfactant.
As one of the preferable modes of the present invention, the initiator a is specifically one of potassium persulfate, ammonium persulfate, and sodium persulfate.
As one of the preferred modes of the invention, the initiator B is specifically sodium thiosulfate or sodium sulfite.
As one of the preferable modes of the present invention, the water absorption accelerator C is specifically sodium dodecyl sulfate.
In the step (2), the addition amounts of the initiator a, the initiator B and the water absorption accelerator C are respectively 0.2 to 0.3% of the acrylic acid raw material.
In the step (3), the reaction time of the materials in the extruder is controlled by adjusting the rotating speed of the extruder screw.
In the step (4), the anti-sticking agent is formed by mixing deionized water, a surface-speaking agent, liquid paraffin and butyl oleate according to a mass ratio of 100:2:10:3.
In the step (4), the size of the colloidal particles after dicing is 3-5 mm; in the step (5), the size of the finely crushed colloidal particles is 40-120 meshes.
Compared with the prior art, the invention has the advantages that:
(1) In the invention, an initiator A, an initiator B and a water absorption accelerator C are added in the polymerization reaction process; under the synergistic effect of the three reagents, the polymerization reaction is more complete, the reaction time is greatly shortened, the polymerization reaction can be completed within 1-5 min, and the production efficiency of the high water absorbent resin is greatly improved; meanwhile, the initiator A, the initiator B and the water absorption accelerator C can also improve the water absorption of the resin to a certain extent, so that the application value of the resin is greatly improved;
(2) The invention installs orifice plate type die head at the outlet of the extruder head; extruding the polymerized sizing material into a linear shape through a head opening die of an extruder, and cutting into colloidal particles at a granulator at the head; compared with the traditional method, the invention extrudes the gelatinous substance after the polymerization reaction into the shape of the linear adhesive tape, and can greatly reduce the time of granulating during the subsequent granulating operation, thereby improving the production efficiency of the super absorbent resin;
(3) In the granulating process, the anti-sticking agent is sprayed outside the surface of the colloidal particle, so that the adhesion of the colloidal particle can be effectively prevented; wherein, the anti-sticking agent is compounded by deionized water, a surface-speaking agent, liquid paraffin and butyl oleate, and when the anti-sticking agent is attached to the surface of the super absorbent resin colloidal particles, the purposes of improving the fluidity of the super absorbent resin and avoiding the adhesion of the colloidal particles can be achieved.
Detailed Description
The following describes in detail the examples of the present invention, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of protection of the present invention is not limited to the following examples.
Example 1
The novel production method of the super absorbent resin comprises the following steps:
(1) Firstly, adding acrylic acid into a reaction kettle, then, dropwise adding sodium hydroxide for neutralization, wherein the reaction temperature is 20 ℃, and the reaction time is 3 hours.
(2) Adding potassium persulfate into the reaction kettle after the neutralization reaction, adding sodium thiosulfate after the mixing is finished, and finally adding sodium dodecyl sulfate for mixing; and in the mixing process, controlling the temperature of the reaction kettle to be not more than 40 ℃.
(3) And (3) adding the mixture into an extruder which is kept at a constant temperature of 70 ℃ to carry out polymerization reaction for 5min after the materials in the step (2) are fully and uniformly mixed.
(4) An orifice plate type die head is arranged at the outlet of the machine head of the extruder; extruding the polymerized sizing material into a linear shape through a head opening die of an extruder, and cutting into 3mm colloidal particles at a granulator at the head; wherein, in the process of granulating, anti-sticking agent is sprayed outside the surface of the colloidal particles to prevent the colloidal particles from adhesion.
(5) The cut particles were dried at 140℃and then finely pulverized into 40-mesh super absorbent resin products.
Further, in this example, in the step (1), the total amount of sodium hydroxide added was 70% of acrylic acid, and the neutralization degree was controlled to be 70%.
In the step (2), the addition amounts of potassium persulfate, sodium thiosulfate and sodium dodecyl sulfate were respectively 0.2% of the acrylic acid raw material.
Further, in the embodiment, in the step (3), the reaction time of the materials in the extruder is controlled by adjusting the rotation speed of the extruder screw.
Further, in the embodiment, in the step (4), the anti-adhesion agent is specifically formed by mixing deionized water, a surface-speaking agent, liquid paraffin and butyl oleate according to a mass ratio of 100:2:10:3.
Example 2
The novel production method of the super absorbent resin comprises the following steps:
(1) Firstly, adding acrylic acid into a reaction kettle, then, dropwise adding sodium hydroxide for neutralization, wherein the reaction temperature is 35 ℃, and the reaction time is 2 hours.
(2) Adding ammonium persulfate into a reaction kettle after the neutralization reaction, adding sodium sulfite after the completion of the mixing, and finally adding sodium dodecyl sulfate for mixing; and in the mixing process, controlling the temperature of the reaction kettle to be not more than 40 ℃.
(3) And (3) adding the mixture into an extruder which is kept at a constant temperature of 80 ℃ to carry out polymerization reaction for 3min after the materials in the step (2) are fully and uniformly mixed.
(4) An orifice plate type die head is arranged at the outlet of the machine head of the extruder; extruding the polymerized sizing material into a linear shape through a head opening die of an extruder, and cutting into 4mm colloidal particles at a granulator at the head; wherein, in the process of granulating, anti-sticking agent is sprayed outside the surface of the colloidal particles to prevent the colloidal particles from adhesion.
(5) The cut particles were dried at 155℃and then finely pulverized into 80-mesh super absorbent resin products.
Further, in this example, in the step (1), the total amount of sodium hydroxide added was 80% of acrylic acid, and the neutralization degree was controlled to 80%.
In the step (2), the addition amounts of ammonium persulfate, sodium sulfite and sodium dodecyl sulfate were respectively 0.25% of the acrylic acid raw material.
Further, in the embodiment, in the step (3), the reaction time of the materials in the extruder is controlled by adjusting the rotation speed of the extruder screw.
Further, in the embodiment, in the step (4), the anti-adhesion agent is specifically formed by mixing deionized water, a surface-speaking agent, liquid paraffin and butyl oleate according to a mass ratio of 100:2:10:3.
Example 3
The novel production method of the super absorbent resin comprises the following steps:
(1) Firstly, adding acrylic acid into a reaction kettle, then, dropwise adding sodium hydroxide for neutralization, wherein the reaction temperature is 45 ℃, and the reaction time is 1.5h.
(2) Adding sodium persulfate into the reaction kettle after the neutralization reaction, adding sodium thiosulfate after the mixing is finished, and finally adding sodium dodecyl sulfate for mixing; and in the mixing process, controlling the temperature of the reaction kettle to be not more than 40 ℃.
(3) And (3) adding the mixture into an extruder which is kept at a constant temperature of 90 ℃ to carry out polymerization reaction for 1min after the materials in the step (2) are fully and uniformly mixed.
(4) An orifice plate type die head is arranged at the outlet of the machine head of the extruder; extruding the polymerized sizing material into a linear shape through a head opening die of an extruder, and cutting into 5mm colloidal particles at a granulator at the head; wherein, in the process of granulating, anti-sticking agent is sprayed outside the surface of the colloidal particles to prevent the colloidal particles from adhesion.
(5) The cut particles are dried at 170 ℃ and then finely crushed into a 120-mesh super absorbent resin product.
Further, in this example, in the step (1), the total amount of sodium hydroxide added was 85% of acrylic acid, and the neutralization degree was controlled to be 85%.
In the step (2), the addition amounts of sodium persulfate, sodium thiosulfate and sodium dodecyl sulfate were 0.3% of the acrylic acid raw material, respectively.
Further, in the embodiment, in the step (3), the reaction time of the materials in the extruder is controlled by adjusting the rotation speed of the extruder screw.
Further, in the embodiment, in the step (4), the anti-adhesion agent is specifically formed by mixing deionized water, a surface-speaking agent, liquid paraffin and butyl oleate according to a mass ratio of 100:2:10:3.
In one of the above examples 1 to 3, an initiator A, an initiator B and a water absorption accelerator C are added during the polymerization reaction; under the synergistic effect of the three reagents, the polymerization reaction is more complete, the reaction time is greatly shortened, the polymerization reaction can be completed within 1-5 min, and the production efficiency of the high water absorbent resin is greatly improved; meanwhile, the initiator A, the initiator B and the water absorption accelerator C can also improve the water absorption of the resin to a certain extent, and greatly improve the application value of the resin.
Secondly, an orifice plate type die head is arranged at the outlet of the machine head of the extruder; extruding the polymerized sizing material into a linear shape through a head opening die of an extruder, and cutting into colloidal particles at a granulator at the head; compared with the traditional method, the invention extrudes the gelatinous substance after the polymerization reaction into the shape of the linear adhesive tape, and can greatly reduce the time of granulating during the subsequent granulating operation, thereby improving the production efficiency of the super absorbent resin.
Thirdly, in the granulating process, the anti-sticking agent is sprayed outside the surface of the colloidal particle, so that the adhesion of the colloidal particle can be effectively prevented; wherein, the anti-sticking agent is compounded by deionized water, a surface-speaking agent, liquid paraffin and butyl oleate, and when the anti-sticking agent is attached to the surface of the super absorbent resin colloidal particles, the purposes of improving the fluidity of the super absorbent resin and avoiding the adhesion of the colloidal particles can be achieved.
Example 4
This example was conducted to test the water absorption properties of the super absorbent resins produced in examples 1 to 3.
The testing method comprises the following steps: adopting a saturated water absorption capacity measuring method; putting 0.5g of the super absorbent resin into a 1000mL beaker, and adding 1000mL of deionized water; after 24 hours, filtering free water by a 140-mesh screen, thoroughly filtering the free water, wiping the bottom of the screen with a dry cotton towel to remove water, weighing the gel weight G, and calculating the water absorption multiple as follows: multiple= (G-0.5) * 2。
The test results are shown in Table 1.
TABLE 1 Water absorption test results of the inventive superabsorbent resin
| Test sample | Example 1 | Example 2 | Example 3 |
| Water absorption multiple | 700 times | 850 times of | 750 times |
As shown in Table 1, the super absorbent resins obtained by the method of the present invention all show good water absorption properties. Among them, the resin obtained in example 2 was the most excellent in water absorption.
Example 5
This example was used to test the flowability of the pellets obtained in examples 1 to 3.
The testing method comprises the following steps: 100g of the granulated colloidal particles with the anti-sticking agent obtained in examples 1 to 3 were added to a glass funnel, the mouth below the funnel was closed with a finger, a stopwatch was pressed down while releasing the finger, and the running-out time of 100g of the colloidal particles was used as an index for measuring the fluidity, and the shorter the time was, the better the fluidity was.
The test results are shown in Table 2.
TABLE 2 results of the particle flowability test of the particle-cut pellets with the anti-sticking agent of the present invention
| Test conditions | Example 1 | Example 2 | Example 3 |
| 100g colloidal particle run-out time(s) | 57 | 30 | 48 |
| Adhesion conditions | Without any means for | Completely loosen | Without any means for |
As can be seen from Table 2, the colloidal particles obtained by the method of the invention have good fluidity and are not easy to adhere. Among them, the colloidal particles obtained by the method of example 2 had the best fluidity, and were the best solutions.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (7)
1. The production method of the super absorbent resin is characterized by comprising the following steps:
(1) Firstly, adding acrylic acid into a reaction kettle, and then, dropwise adding sodium hydroxide for neutralization; the reaction temperature of the neutralization reaction is 20-45 ℃ and the reaction time is 1.5-3 h;
(2) Adding an initiator A into a reaction kettle after the neutralization reaction, adding an initiator B after the mixing, and finally adding a water absorption accelerator C for mixing; the temperature of the reaction kettle is controlled to be not more than 40 ℃ in the mixing process; wherein the initiator A is peroxide, the initiator B is a reducing substance, and the water absorption promoter C is sodium dodecyl sulfate;
(3) After the materials in the step (2) are fully and uniformly mixed, adding the mixture into an extruder which is kept at a constant temperature of 70-90 ℃ for polymerization reaction for 1-5 min;
(4) An orifice plate type die head is arranged at the outlet of the machine head of the extruder; extruding the polymerized sizing material into a linear shape through a head opening die of an extruder, and cutting into colloidal particles at a granulator at the head; wherein, during the grain cutting process, anti-sticking agent is sprayed outside the surface of the colloidal particle to prevent the colloidal particle from adhesion; the anti-sticking agent is prepared by mixing deionized water, a surfactant, liquid paraffin and butyl oleate according to a mass ratio of 100:2:10:3;
(5) Drying the cut particles at 140-170 ℃, and then finely crushing the particles into the target super absorbent resin product.
2. The method for producing a superabsorbent resin according to claim 1, wherein in the step (1), the total amount of sodium hydroxide added is 70 to 85% of acrylic acid, and the neutralization degree is controlled to be 70 to 85%.
3. The method for producing a super absorbent resin according to claim 1, wherein the initiator a is specifically one of potassium persulfate, ammonium persulfate, and sodium persulfate.
4. The method for producing a super absorbent resin according to claim 1, wherein the initiator B is specifically sodium thiosulfate or sodium sulfite.
5. The method for producing a super absorbent resin according to claim 1, wherein in the step (2), the addition amounts of the initiator a, the initiator B and the water absorption accelerator C are respectively 0.2 to 0.3% of the acrylic acid raw material.
6. The method for producing a super absorbent resin according to claim 1, wherein in the step (3), the reaction time of the materials therein is controlled by adjusting the rotation speed of the extruder screw.
7. The method for producing a super absorbent resin according to claim 1, wherein in the step (4), the size of the colloidal particles after dicing is 3 to 5mm; in the step (5), the size of the finely crushed colloidal particles is 40-120 meshes.
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