CN111304920A - Water-absorbing resin solution, preparation method and preparation method of water-blocking glass fiber yarn - Google Patents
Water-absorbing resin solution, preparation method and preparation method of water-blocking glass fiber yarn Download PDFInfo
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Abstract
A water-absorbent resin solution is prepared by mixing the following components in parts by mass: 20-100 parts of water; 4-8 parts of sodium hydroxide; 10-20 parts of acrylic acid; 4-10 parts of acrylamide; 0.003 to 0.01 portion of cross-linking agent; 0.1-0.4 part of initiator; 1-5 parts of polyvinyl alcohol and/or 1-5 parts of polyvinylpyrrolidone. The neutralization reaction of acrylic acid and sodium hydroxide generates sodium acrylate and water, the acrylic acid is excessive, and the sodium acrylate, the rest acrylic acid and acrylamide are subjected to polymerization and crosslinking reaction under the high-temperature conditions of an initiator and a crosslinking agent to generate a crosslinked polymer with a three-dimensional network structure, so that the adhesive has strong adhesion. After the glass fiber yarns are soaked in the water-absorbent resin solution and dried, the water-absorbent resin can be adhered to the surfaces of the glass fibers, and for the glass fiber yarns formed by gathering a large number of glass fibers, the water-absorbent resin is adhered to the inner parts and the surfaces of the glass fiber yarns, so that the water-blocking effect is more excellent, the tensile property and the like are improved, and the powder cannot fall off in the using process.
Description
Technical Field
The invention relates to the technical field of glass fiber yarns, in particular to a water-absorbent resin solution, a preparation method and a preparation method of water-blocking glass fiber yarns.
Background
The glass fiber is an inorganic non-metallic material with excellent performance, has various types, has the advantages of good insulativity, strong heat resistance, good corrosion resistance and high mechanical strength, and is usually used as a reinforcing material, an electrical insulating material and a heat insulation material in a composite material.
With the rapid development of the communication industry in China, the performance requirements of optical cables are continuously improved. The water blocking performance of optical cables is one of the important criteria. The filling water-blocking material for the optical cable is developed to the present day, and the filling water-blocking material mainly comprises two types: one is ointment; the other is water-blocking tape, water-blocking yarn and water-blocking glass fiber yarn. Ointment water blocking is a very traditional filling waterproof means, and along with the development of dry optical cables, water blocking glass fiber yarns are increasingly applied to the production of optical cables.
For example, in the invention patent application with the application publication number of CN103061136A, a glass fiber yarn for water blocking of optical cable and a manufacturing process thereof are disclosed, wherein an abrasion-resistant coating layer is formed on a raw material glass fiber yarn through high-temperature cross-linking polymerization to form an abrasion-resistant glass fiber yarn, and then a hydrophilic expansion coating layer is formed on the surface of the abrasion-resistant glass fiber yarn through high-temperature cross-linking polymerization to obtain the glass fiber yarn for water blocking of optical cable. The water-blocking glass fiber yarn is not easy to transversely break, has excellent hydrophilic expansion performance, can enhance the tensile resistance of the optical cable, and the optical cable manufactured by the water-blocking glass fiber yarn has the advantages of metal-free structure, oil-free structure, simple use, good water-blocking performance, light weight, resource saving and no pollution.
The infiltration process is carried out in two steps, so the production process is more complicated and the production efficiency is lower.
Disclosure of Invention
The first object of the present invention is to provide a resin absorbent solution which is advantageous in that the adhesion of powder after the water absorbent resin is easily dried is good and the water absorption swelling rate is high.
The above object of the present invention is achieved by the following technical solutions:
a water-absorbent resin solution is prepared by mixing the following components in parts by mass:
1-5 parts of polyvinyl alcohol and/or 1-5 parts of polyvinylpyrrolidone.
By adopting the technical scheme, the neutralization reaction of acrylic acid and sodium hydroxide generates sodium acrylate and water: c3H4O2+NaOH→C3H3NaO2+H2And O, drying the glass fiber yarns in the soaked water-absorbent resin solution in an oven, wherein in the drying process, excessive acrylic acid is used, and sodium acrylate, residual acrylic acid and acrylamide are subjected to polymerization and crosslinking reaction under the high-temperature conditions of an initiator and a crosslinking agent to generate a crosslinked polymer with a three-dimensional network structure, so that the glass fiber yarns have strong adhesion. After drying, the water-absorbent resin is only adhered to the surface of the glass fiber tightly, and for the glass fiber yarn formed by gathering a large number of glass fibers, the water-absorbent resin is adhered to the inner part and the surface of the glass fiber yarn, so that the water-blocking effect is more excellent, the tensile property and the like are improved, and the powder cannot fall off in the using process, therefore, the water-absorbent resin is beneficial to protecting the physical health and the environmental sanitation of personnel in the whole production, transportation and use process, and has great significance for the production and development of optical cables.
The polyvinylpyrrolidone has good cohesiveness and hygroscopicity, so that after being added into a resin solution, the cohesiveness and hygroscopicity of the dried resin can be obviously improved, meanwhile, under the action of high-temperature crosslinking, polyvinyl alcohol and/or polyvinylpyrrolidone and residual acrylic acid can be complexed to a certain extent to participate in the generation of a crosslinked polymer with a three-dimensional network structure, and meanwhile, after the polyvinylpyrrolidone and the polyvinyl alcohol are mixed, the polyvinyl alcohol can be effectively dispersed, so that the physical and chemical properties of all parts of the resin are uniform and stable, the integrity and completeness of the resin are improved, and the powder falling phenomenon of glass fiber yarns is further reduced.
Preferably, the polyvinyl alcohol is one or more of PVA17-88, PVA17-92, PVA17-99, PVA20-99, PVA23-99, PVA24-88 and PVA 26-99.
Preferably, the crosslinking agent is one or more of N, N-methylene bisacrylamide, polyethylene glycol and polyethylene glycol diacrylate.
Preferably, the polyethylene glycol is one or more of PEG2000, PEG5000 and PEG 10000.
Preferably, the polyethylene glycol diacrylate is one or more of PEG200DA, PEG400DA and PEG600 DA.
Preferably, the initiator is one or more of potassium persulfate, ammonium persulfate and sodium bisulfite.
By adopting the technical scheme, potassium sulfate, ammonium persulfate and sodium bisulfite are taken as the initiator, and sodium acrylate, the rest acrylic acid and acrylamide are subjected to polymerization and crosslinking reaction under the high-temperature conditions of the initiator and the crosslinking agent.
The second object of the present invention is to provide a method for producing a water absorbent resin solution.
A preparation method of a water-absorbent resin solution specifically comprises the following steps:
s1, adding water into the reaction kettle, and starting stirring and high-low temperature circulation;
s2, adding acrylic acid into the reaction kettle, and keeping the temperature at 20 +/-5 ℃;
s3, dropwise adding the prepared sodium hydroxide solution into the reaction kettle;
s4, after the reaction is completed, adding acrylamide, a cross-linking agent and an initiator, and uniformly stirring to obtain a primary solution;
s5, mixing the polyvinyl alcohol, the polyvinylpyrrolidone and the preliminary solution of S4 which are dissolved in water in advance to obtain the aqueous polymer water-absorbent resin solution.
By adopting the technical scheme, water is added into the reaction kettle, and stirring and high-low temperature circulation are started to prepare for the continuous preparation of the resin solution; adding acrylic acid, gradually dissolving sodium hydroxide in water, gradually increasing the temperature of the solution, ensuring the final temperature of the acrylic acid solution to be 20 +/-5 ℃ through high-low temperature circulation, and fully reacting the acrylic acid with the sodium hydroxide solution; continuously adding acrylamide, a cross-linking agent, an initiator and polyvinyl alcohol/polyvinylpyrrolidone, and carrying out polymerization cross-linking reaction under the high-temperature drying condition to generate a cross-linked polymer with a three-dimensional network structure.
Since acrylic acid is easy to self-polymerize at high temperature (above 25 ℃) and easily coagulate at low temperature (below 15 ℃), the acrylic acid is finally maintained at 20 +/-5 ℃, so that the acrylic acid can be reacted with the sodium hydroxide solution as thoroughly as possible after the sodium hydroxide solution is dripped, rather than self-polymerizing or coagulating, and the reaction efficiency is improved.
Preferably, in S3, the temperature of the mixed solution in the reaction kettle is kept at 20. + -. 5 ℃ all the time.
By adopting the technical scheme, the reaction of acrylic acid and sodium hydroxide is an acid-base reaction, so that the exothermic phenomenon can be generated, and the acrylic acid is dripped into the sodium hydroxide solution, so that the temperature of the solution can be conveniently controlled, and the stability of the temperature can be kept.
In the whole process of dropwise adding the sodium hydroxide solution, the temperature needs to be kept at 20 +/-5 ℃ to prevent the acrylic acid from self-polymerization, so that the acrylic acid can be further ensured to react with the sodium hydroxide solution as thoroughly as possible; meanwhile, the excessive acrylic acid can also ensure that the acrylic acid is in a stable dissolved state, thereby facilitating the continuous operation of subsequent reaction.
The third purpose of the invention is to provide a preparation method of the water-blocking glass fiber yarn.
A preparation method of water-blocking glass fiber yarns comprises the steps of immersing the glass fiber yarns into water-absorbent resin solution for soaking, and drying the glass fiber yarns soaked with the water-absorbent resin solution.
By adopting the technical scheme, the glass fiber yarns are immersed in the water-absorbent resin solution, so that the water-absorbent resin solution can be fully distributed on the glass fiber yarns as much as possible, and after drying, the water-absorbent resin is adhered on the glass fiber yarns, thereby forming the water-swelling water-blocking glass fiber yarns. The whole process can be completed only by one-step infiltration, the production steps are simple, and the production efficiency is high.
In conclusion, the beneficial technical effects of the invention are as follows:
1. the polyvinyl alcohol can be dissolved in the water solution at 60-80 ℃, and can be coagulated at normal temperature, so that after the polyvinyl alcohol is added into the solution and the resin solution is restored to the room temperature, the resin can be better shaped so as to be adhered to the glass fiber, and the powder falling of the glass fiber yarn is reduced;
2. the polyvinylpyrrolidone can obviously improve the caking property and the hygroscopicity of the dried resin, and can be complexed with the residual acrylic acid to a certain extent under the action of high-temperature crosslinking, and can be effectively dispersed after being mixed with the polyvinyl alcohol, so that the physical and chemical properties of the resin are uniform and stable, the integrity and the completeness of the resin are improved, and the powder falling phenomenon of the glass fiber yarn is further reduced.
Drawings
FIG. 1 is a diagram showing a process for preparing a water absorbent resin solution.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The various raw materials used in the present application are commercially available chemical raw materials.
Firstly, preparing a water-absorbent resin solution and water-blocking glass fiber yarns:
the invention discloses a water-absorbent resin solution which is prepared by mixing the following components in parts by mass:
wherein, the polyvinyl alcohol is one or more of PVA17-88, PVA17-92, PVA17-99, PVA20-99, PVA23-99, PVA24-88 and PVA 26-99.
Wherein the cross-linking agent is one or more of N, N-methylene bisacrylamide, polyethylene glycol and polyethylene glycol diacrylate.
Wherein the polyethylene glycol is one or more of PEG2000, PEG5000 and PEG 10000.
Wherein the polyethylene glycol diacrylate is one or more of PEG200DA, PEG400DA and PEG600 DA.
Wherein the initiator is one or more of potassium persulfate, ammonium persulfate and sodium bisulfite.
Referring to the attached figure 1, the preparation method of the aqueous polymer water-absorbent resin solution comprises the following steps:
s1, adding water into the reaction kettle, and starting stirring and high-low temperature circulation;
s2, adding acrylic acid into the reaction kettle, and keeping the temperature at 20 +/-5 ℃;
s3, dropwise adding the prepared sodium hydroxide solution into the reaction kettle;
s4, after the reaction is completed, adding acrylamide, a cross-linking agent and an initiator, and uniformly stirring to obtain a primary solution;
s5, mixing the polyvinyl alcohol, the polyvinylpyrrolidone and the preliminary solution of S4 which are dissolved in water in advance to obtain the aqueous polymer water-absorbent resin solution.
Examples 1,
S1, preparation of the aqueous high-molecular water-absorbent resin solution: weighing 70 parts of deionized water, adding the deionized water into a reaction kettle, starting stirring and high-low temperature circulation, and controlling the temperature at 20 ℃;
s2, adding 12 parts of acrylic acid, and stirring in a reaction kettle;
s3, stirring the solution in the step S2 for 30 minutes, after the temperature returns to 20 ℃, dropwise adding 5 parts of sodium hydroxide, and keeping the temperature at 20 ℃ in the process;
and S4, adding 6 parts of acrylamide, 0.005 part of cross-linking agent and 0.1 part of initiator after 1 hour, and stirring for 30min to obtain a primary solution.
S5, mixing 3 parts of polyvinyl alcohol solution dissolved in water in advance with the preliminary solution of S4 to obtain the aqueous macromolecular water-absorbent resin solution.
Wherein the cross-linking agent is N, N-methylene bisacrylamide; the polyvinyl alcohol is PVA 17-88; the initiator is potassium persulfate.
Examples 2,
S1, preparation of the aqueous high-molecular water-absorbent resin solution: weighing 80 parts of deionized water, adding the deionized water into a reaction kettle, starting stirring and high-low temperature circulation, and controlling the temperature at 25 ℃;
s2, adding 14 parts of acrylic acid, and stirring in a reaction kettle;
s3, stirring the solution in the step S2 for 30 minutes, after the temperature returns to 25 ℃, dropwise adding 6 parts of sodium hydroxide, and keeping the temperature at about 25 ℃ in the process;
s4, adding 7 parts of acrylamide, 0.006 part of cross-linking agent and 0.3 part of initiator after 1 hour, and uniformly stirring to obtain a primary solution;
s5, mixing 3 parts of polyvinylpyrrolidone solution dissolved in water in advance with the preliminary solution of S4 to obtain the aqueous macromolecular water-absorbent resin solution.
Wherein the cross-linking agent is PEG2000 polyethylene glycol; the polyvinyl alcohol is a mixture of PVA20-99, PVA23-99, PVA24-88 and PVA26-99 in a mass ratio of 1:1:1: 1; the initiator is a mixture of ammonium persulfate and sodium bisulfite with the mass ratio of 1: 1.
Examples 3,
S1, preparation of the aqueous high-molecular water-absorbent resin solution: weighing 80 parts of deionized water, adding the deionized water into a reaction kettle, starting stirring and high-low temperature circulation, and controlling the temperature at 25 ℃;
s2, adding 14 parts of acrylic acid, and stirring in a reaction kettle;
s3, stirring the solution in the step S2 for 30 minutes, after the temperature returns to 25 ℃, dropwise adding 5 parts of sodium hydroxide, and keeping the temperature at about 15 ℃ in the process;
s4, adding 8 parts of acrylamide, 0.01 part of cross-linking agent and 0.4 part of initiator after 1 hour, and uniformly stirring to obtain a primary solution;
s5, mixing 2 parts of polyvinyl alcohol dissolved in water in advance, 1 part of polyvinylpyrrolidone solution and the preliminary solution of S4 to obtain the water-based high-molecular water-absorbent resin solution.
Wherein the cross-linking agent is a mixture of PEG200DA polyethylene glycol diacrylate, PEG400DA polyethylene glycol diacrylate and the mass ratio of 1: 1; the polyvinyl alcohol is a mixture of PVA17-92 and PVA17-99 in a mass ratio of 1: 1; the initiator is a mixture of potassium persulfate, ammonium persulfate and sodium bisulfite in a mass ratio of 1:1: 1.
Examples 4,
S1, preparation of the aqueous high-molecular water-absorbent resin solution: weighing 20 parts of deionized water, adding into a reaction kettle, starting stirring and high-low temperature circulation, and controlling the temperature at 15 ℃;
s2, adding 10 parts of acrylic acid, and stirring and dissolving in a reaction kettle;
s3, stirring the dissolved solution in the step S2 for 30 minutes, after the temperature returns to 25 ℃, dropwise adding 4 parts of sodium hydroxide, and keeping the temperature at 25 ℃ in the process;
s4, adding 4 parts of acrylamide, 0.003 part of cross-linking agent and 0.1 part of initiator after 1 hour, and uniformly stirring to obtain a primary solution;
s5, mixing 1 part of polyvinyl alcohol and 1 part of polyvinylpyrrolidone solution which are dissolved in water in advance with the preliminary solution of S4 to obtain the water-based high-molecular water-absorbent resin solution.
Wherein the cross-linking agent is a mixture of PEG200DA polyethylene glycol diacrylate, PEG400DA polyethylene glycol diacrylate and PEG600DA polyethylene glycol diacrylate in a mass ratio of 1:1: 1; the polyvinyl alcohol is PVA 17-92; the initiator is a mixture of potassium persulfate and sodium bisulfite with the mass ratio of 1: 1.
Examples 5,
S1, preparation of the aqueous high-molecular water-absorbent resin solution: weighing 100 parts of deionized water, adding the deionized water into a reaction kettle, starting stirring and high-low temperature circulation, and controlling the temperature at 25 ℃;
s2, adding 20 parts of acrylic acid, and stirring and dissolving in a reaction kettle;
s3, stirring the dissolved solution in the step S2 for 30 minutes, after the temperature returns to 25 ℃, dropwise adding 8 parts of sodium hydroxide, and keeping the temperature at 25 ℃ in the process;
s4, adding 10 parts of acrylamide, 0.01 part of cross-linking agent and 0.4 part of initiator after 1 hour, and uniformly stirring to obtain a primary solution; s5, mixing 5 parts of polyvinyl alcohol and 5 parts of polyvinylpyrrolidone solution which are dissolved in water in advance with the preliminary solution of S4 to obtain the water-based high-molecular water-absorbent resin solution.
Wherein the cross-linking agent is PEG200DA polyethylene glycol diacrylate; the polyvinyl alcohol is a mixture of PVA17-92, PVA17-99 and PVA20-99 in a mass ratio of 1:1: 1; the initiator is a mixture of potassium persulfate, ammonium persulfate and sodium bisulfite in a mass ratio of 1:1: 1.
II, test testing:
1. testing yarn sample linear density:
taking a glass yarn sample with the length of 10m by using a precision roller, wherein the length is recorded as L, weighing the glass yarn sample on a balance, and the mass is recorded as m; the glass yarn density LD ═ 1000 xm/L was determined according to the formula.
As can be seen from the above table, the linear densities of examples 1 to 5 are all in the range of 600 ± 5% tex, so that the linear density of the glass fiber yarn is more stable, and compared with the glass fiber yarn in the patent application with application publication No. CN10361136A, the linear density stability of the glass fiber yarn in the present application is stronger, and the actual density of the cable is easier to control and the operation is convenient after the cable is added in the actual use process.
2. And (3) testing the water absorption rate of the solution:
drying a proper amount of aqueous macromolecular water-absorbent resin solution in an oven at the temperature of between 80 and 120 ℃; crushing the dried sample, taking out the crushed sample, putting the crushed sample into a 160-mesh test sieve, shaking the test sieve for 5-10min, sieving the powdery sample, and taking the sieved powder (fine powder) as a test sample; putting 1000ml of purified water into a 1000ml beaker or a measuring cylinder; weighing 1.00g of sample m0, slowly adding the sample m0 into water, taking care to avoid agglomeration of fine powder, and starting timing to ensure that the sample is fully saturated with water; pouring the water-absorbed gel into a test sieve with a weighed weight of m1 after 30min, washing a beaker or a measuring cylinder with a small amount of water, merging into the test sieve, standing and filtering; after filtering for 1h, observing whether water drops are dropped on the lower part of the test sieve, and weighing and reading the weight m2 of the test sieve and the gel if no water drops are continuously dropped. And calculating the water absorption expansion ratio of the water-blocking solution according to the formula of (m2-m1-m0)/m 0.
3. And (3) testing the water absorption expansion rate of the water-blocking glass yarn:
testing was performed according to standard YD/T1181.4-2015;
a piece of yarn was weighed m0, and a dry 200ml beaker was weighed m1 to the nearest 0.1 g. The weighed yarn was placed in another 200ml beaker with purified (or deionized) water. After soaking in water for 30s, the sample was removed with tweezers, drained for 30s and placed in a weighed beaker, and weighed to the nearest 0.1g m 2.
The yarn swell rate was calculated according to the formula X1 ═ m2-m1-m0)/m 0.
4. And (3) testing the water absorption expansion multiplying power of the water-blocking glass yarn:
testing was performed according to standard YD/T1181.4-2015;
a piece of yarn was weighed m0, and a dry 200ml beaker was weighed m1 to the nearest 0.1 g. The weighed yarn was placed in another 200ml beaker with purified (or deionized) water. After soaking in water for 5min, the sample was removed with tweezers, drained for 30s and placed in a weighed beaker, and weighed to the nearest 0.1g m 2.
The yarn swell ratio was calculated according to the formula X2 ═ m2-m1-m0)/m 0.
Compared with the glass fiber yarn disclosed in the patent application with the application publication number of CN10361136A, the water-blocking glass yarn disclosed by the application has the advantage that the water absorption expansion multiplying power is improved by 120%, so that the water-blocking glass yarn has better water absorption expansion property, and the water-blocking performance is obviously improved.
5. Other performance tests:
the tests were carried out with reference to the standard YD/T1181.4-2015:
therefore, it can be seen from the above experimental data that after the glass fiber yarn is soaked in the water-absorbent resin solution and dried, the water-absorbent resin will only adhere to the surface of the glass fiber yarn, so as to form the water-blocking glass fiber yarn which is water-swellable, and therefore, the water-blocking glass fiber yarn has a better water-blocking effect, is improved in tensile properties and the like, and will not fall off during use.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (9)
1. A water-absorbent resin solution characterized by: the paint is prepared by mixing the following components in parts by mass:
20-100 parts of water;
4-8 parts of sodium hydroxide;
10-20 parts of acrylic acid;
4-10 parts of acrylamide;
0.003 to 0.01 portion of cross-linking agent;
0.1-0.4 part of initiator;
1-5 parts of polyvinyl alcohol and/or 1-5 parts of polyvinylpyrrolidone.
2. The water absorbent resin solution according to claim 1, characterized in that: the polyvinyl alcohol is one or more of PVA17-88, PVA17-92, PVA17-99, PVA20-99, PVA23-99, PVA24-88 and PVA 26-99.
3. The water absorbent resin solution according to claim 1, characterized in that: the cross-linking agent is one or more of N, N-methylene bisacrylamide, polyethylene glycol and polyethylene glycol diacrylate.
4. The water absorbent resin solution according to claim 3, characterized in that: the polyethylene glycol is one or more of PEG2000, PEG5000 and PEG 10000.
5. The water absorbent resin solution according to claim 3, characterized in that: the polyethylene glycol diacrylate is one or more of PEG200DA, PEG400DA and PEG600 DA.
6. The water absorbent resin solution according to claim 1, characterized in that: the initiator is one or more of potassium persulfate, ammonium persulfate and sodium bisulfite.
7. A method for preparing a water-absorbent resin solution, which is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, adding water into the reaction kettle, and starting stirring and high-low temperature circulation;
s2, adding acrylic acid into the reaction kettle, and keeping the temperature at 20 +/-5 ℃;
s3, dropwise adding the prepared sodium hydroxide solution into the reaction kettle;
s4, after the reaction is completed, adding acrylamide, a cross-linking agent and an initiator, and uniformly stirring to obtain a primary solution;
s5, mixing the polyvinyl alcohol, the polyvinylpyrrolidone and the preliminary solution of S4 which are dissolved in water in advance to obtain the aqueous polymer water-absorbent resin solution.
8. The method for self-preparation of a water-absorbent resin solution according to claim 7, characterized in that: in S3, the temperature of the mixed solution in the reaction kettle is kept at 20 +/-5 ℃.
9. A preparation method of water-blocking glass fiber yarn is characterized by comprising the following steps: soaking the glass fiber yarns in the water-absorbent resin solution, and drying the glass fiber yarns soaked with the water-absorbent resin solution.
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