Preparation process and application of flexible thickening agent

Abstract

The invention provides a preparation process and application of a flexible thickening agent, and relates to the technical field of thickening agent preparation, the preparation process comprises the following steps: preparing a thickening agent and industrial water into white slurry samples with different thickening agent contents and concentrations, respectively measuring the white slurry viscosities of different samples by using a rotary viscometer, and respectively measuring the viscosities of the samples by using the rotary viscometer; the method comprises the following steps: dissolving a reactive red dye with industrial water to prepare a dye solution with the mass fraction of 0.17%, proportioning the dye solution with a thickening agent to obtain color paste samples with different concentrations in which the content of the thickening agent is different, and respectively measuring the viscosities of the samples by using a rotary viscometer; the technical key points are as follows: a main body with the best viscosity and flexibility in a single field is obtained through a mixing experiment between thickeners with different concentrations and the main body, and the main body with the best viscosity and flexibility in each field is compared, so that a scene with the best use effect under the single concentration of the thickeners can be determined; and the possibility of using a single thickening agent in various fields and the huge progress of the dosage and the use method are favorably obtained, and the research and development cost is reduced.

Description

Technical Field

[0001] The invention relates to the technical field of thickener preparation, in particular to a preparation process and application of a flexible thickener. Background Art

[0002] Thickeners, also known as gelling agents, are substances that can increase the viscosity of latex and liquids. When used in food, they are also called pastes. Thickeners can increase the viscosity of a system, keep the system in a uniform and stable suspended state or emulsified state, or form a gel; most thickeners also have an emulsifying effect. Thickeners are widely used in food (such as adding food additives to sauces, jams, ice cream, canned food, etc. to increase food viscosity or form a gel), cosmetics, detergents, latex, printing and dyeing, medicine, rubber, coatings, etc.

[0003] Thickeners can be divided into two categories: natural and synthetic. Most natural products are made from plants and seaweeds containing polysaccharide viscous substances, such as starch, gum arabic, pectin, agar, gelatin, alginate, carrageenan, dextrin, general gelatin, soluble starch, polysaccharide derivatives, etc. Synthetic products include carboxymethyl cellulose, propylene glycol alginate, methyl cellulose, sodium starch phosphate, sodium carboxymethyl cellulose, sodium alginate, casein, sodium polyacrylate, polyoxyethylene, polyvinyl pyrrolidone, etc.

[0004] The preparation process of existing thickeners is relatively fixed, and the thickener products produced by a single process generally correspond to a single application field. Although the viscosity of the target product can be optimized in the corresponding application scenario by continuously debugging equipment, changing the amount of raw materials and the ratio between the raw materials, it takes repeated tests for the optimal state of a single thickener applied to the target product, and it is difficult to obtain unexpected progress without changing the formula. During the experiment, manpower and material resources are consumed, and it is difficult to obtain practical results for creative breakthroughs in this field. Summary of the invention

[0005] In order to overcome the problem that the preparation process of existing thickeners is relatively fixed, and the thickener products produced by a single process generally correspond to a single application field, it is necessary to repeat multiple tests for the best state of a single thickener applied to a target product, and it is difficult to obtain unexpected progress without changing the formula. In the experimental process, manpower and material resources are consumed, and it is difficult to obtain practical effects for creative breakthroughs in this field. The embodiment of the present application provides a preparation process and application of a flexible thickener. By using the prepared thickener in the main body in different fields, and obtaining the main body with the best viscosity and flexibility in a single field through mixing experiments at different concentrations, and comparing the main bodies with the best viscosity and flexibility in various fields, the best scenario for the use of the thickener at a single concentration can be determined. Referring to the existing method of continuous experimentation and debugging in a single field, a single thickener can be experimented in different fields, and the existing experimental method in a single field can be assisted, which is conducive to obtaining the possibility of obtaining the use of a single thickener in various fields and the huge progress in the dosage and usage of the thickener, and reducing research and development costs.

[0006] The technical solution adopted by the embodiment of the present application to solve the technical problem is:

[0007] A preparation process of a flexible thickener comprises the following steps: taking a container A, dissolving an acrylic acid monomer and a methylpropane sulfonic acid monomer in water, and stirring with the aid of a crosslinking agent and an initiator, thereby obtaining an aqueous phase mixed solvent, which is recorded as a raw material solution A;

[0008] Step 2: Under low temperature, add sodium hydroxide solution to the raw material solution A, and make it reach an acid-base neutralization state under the premise of monitoring the pH value of the raw material solution A by a pH monitor, which is recorded as aqueous phase solution B;

[0009] Step 3: Take container B, and place a certain amount of liquid paraffin, cyclohexane, sorbitan monooleate and stabilizer therein, and stir and mix, to obtain an oil phase solution C after clarification;

[0010] Step 4: Add the aqueous solution B to the oil phase solution C, stir rapidly to make it emulsified completely, and introduce nitrogen to deoxygenate, to obtain a thickener stock solution D;

[0011] Step 5: Raise the temperature of thickener stock solution D to 45 degrees Celsius to initiate the reaction. After the reaction is completed, keep the temperature between 40 degrees Celsius and 43 degrees Celsius for 3 hours, and then heat it to 75 degrees Celsius to react.

[0012] Step 6: reflux the reheated thickener stock solution D for 3 hours, and remove the solvent therein by azeotropic distillation;

[0013] Step 7: Let the dehydrated thickener stock solution D stand until it is at room temperature, then add emulsifier T-80 and stir to gradually change phases to obtain the thickener.

[0014] In a possible implementation, the neutralization degree of the acrylic acid monomer and the methylpropane sulfonic acid monomer in step 1 is 89%-91%.

[0015] In a possible implementation, the ratio of the cross-linking agent used before mixing the raw material solution A in step 1 to the total mass of the monomers (acrylic acid monomer and methylpropane sulfonic acid monomer) is 3:2000.

[0016] In a possible implementation, the ratio of the initiator used before mixing the raw material solution A in step 1 to the total mass of the monomers (acrylic acid monomer and methylpropanesulfonic acid monomer) is 1:1000.

[0017] In a possible implementation, the mass ratio of the emulsifier used in the phase transition of the thickener stock solution D in step seven to the oil phase solution C is 3:25.

[0018] In a possible implementation, the thickener obtained in step seven is mixed with industrial water to prepare five white slurry samples with different concentrations of thickener content of 0.1%, 0.2%, 0.4%, 0.8% and 1.0%, and the white slurry viscosity of the different samples is measured by a rotational viscometer.

[0019] In one possible implementation, the reactive red dye is dissolved in industrial water to prepare a dye solution with a mass fraction of 0.17%, and then the dye solution is mixed with the thickener obtained in step seven to obtain four different concentrations of color paste samples with thickener contents of 2%, 4%, 6% and 8%, and the white paste viscosity of the different samples is measured by a rotational viscometer.

[0020] In a possible implementation, a Na2SO4 salt solution is prepared and mixed with the thickener obtained in step seven, and three white pulp samples with different concentrations of 3%, 4% and 5% thickener content are obtained, and the white pulp viscosity of the different samples is measured by a rotational viscometer.

[0021] In a possible implementation, a composite solution of Na2SO4 and an active substance is prepared and proportioned with the thickener obtained in step seven, and eight white slurry samples with thickener contents of 0.5%, 1%, 1.5%, 2.0%, 2.5%, 3%, 3.5% and 4% are obtained, and the white slurry viscosities of the different samples are measured by a rotational viscometer.

[0022] In one possible implementation, different main surfactants, additives and preservatives in shampoo are selected to form a solution, which is then proportioned with the thickener (secondary surfactant) obtained in step seven, and four white pulp samples with different concentrations of thickener content of 0.5%, 1.0%, 1.5% and 2.0% are obtained, and the white pulp viscosity of different samples is measured by a rotational viscometer.

[0023] The invention discloses an application of a flexible thickener as a printing and dyeing thickener.

[0024] The beneficial effects of this application are:

[0025] First, in this scheme, by using two containers to process the aqueous phase solution and the oil phase solution of the thickener respectively, and under the premise of controlling the percentage of neutralization degree when mixing different monomers, as well as the amount of crosslinking agent, initiator and emulsifier, the aqueous phase solution in one container is mixed with the oil phase solution in another container, and then the thickener is obtained by heating, heat preservation, reheating, heat preservation and phase transfer, so that the viscosity of the thickener can be effectively increased during the application process, and no particles will appear;

[0026] Second, in this scheme, by using the prepared thickener in the main body in different fields, and obtaining the main body with the best viscosity and flexibility in a single field through mixing experiments at different concentrations, and comparing the main bodies with the best viscosity and flexibility in each field, the best scenario for using the thickener at a single concentration can be determined. By referring to the existing method of continuous experimentation and debugging in a single field, a single thickener can be experimented in different fields and assisted in the existing experimental method in a single field, which is conducive to obtaining the possibility of using a single thickener in various fields and a huge improvement in the dosage and usage of the thickener, and reducing R&D costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 This is a schematic diagram of the monomer neutralization degree data in the preparation process of a flexible thickener of the present invention. DETAILED DESCRIPTION

[0028] The technical solution in the embodiment of the present application is to solve the problems of the above-mentioned background technology, and the overall idea is as follows:

[0029] Embodiment 1:

[0030] This embodiment introduces a preparation process of a flexible thickener, comprising S1: taking a container A, dissolving an acrylic acid monomer and a methylpropane sulfonic acid monomer in water, and stirring with the aid of a crosslinking agent and an initiator, thereby obtaining an aqueous phase mixed solvent, which is recorded as a raw material solution A;

[0031] Among them, Figure 1As shown, by setting the neutralization degree of acrylic acid monomer and methylpropane sulfonic acid monomer to between 89% and 91%, the finished thickener can ensure thickening performance and avoid the presence of a large amount of negative charges in the monomer, which leads to poor thickening ability and affects the activity of the cross-linking agent, resulting in a low cross-linking degree of the polymer;

[0032] Secondly, the ratio of the cross-linking agent used before the raw material solution A is mixed to the total mass of the monomers (acrylic acid monomers and methylpropane sulfonic acid monomers) is 3:2000 (i.e., the cross-linking agent is 0.15% of the monomer mass), and the ratio of the initiator used before the raw material solution A is mixed to the total mass of the monomers (acrylic acid monomers and methylpropane sulfonic acid monomers) is 1:1000 (i.e., the initiator is 0.1% of the monomer mass);

[0033] At the same time, a container A (reactor) is used to hold water for preparing raw material solution A, acrylic acid monomer and methylpropane sulfonic acid monomer raw material solution are dissolved in water, and water and monomer (a mixture of acrylic acid monomer and methylpropane sulfonic acid monomer) are mixed with the help of a mixing structure configured in the reactor itself;

[0034] S2: Under low temperature, sodium hydroxide solution is added to the raw material solution A, and the pH value of the raw material solution A is monitored by a pH monitor to achieve an acid-base neutralization state, which is recorded as aqueous solution B;

[0035] Wherein, based on the reaction equipment in S1, the temperature of the reactor is controlled to keep the raw material solution A at a low temperature, and the acidic substances therein are neutralized by the sodium hydroxide solution to make it reach a specified pH state, and the pH is monitored in real time by a pH monitor to control the sodium hydroxide solution, and finally the water phase part of the thickener is obtained;

[0036] S3: Take container B, and place a certain amount of liquid paraffin, cyclohexane, sorbitan monooleate and stabilizer therein, and stir and mix, to obtain an oil phase solution C after clarification;

[0037] Among them, container B (reactor) is used to mix quantitative liquid paraffin, cyclohexane, sorbitan monooleate and stabilizer, and its specific usage amount is adjusted according to the usage amount of each raw material in aqueous solution B and its own total amount;

[0038] S4: adding the aqueous solution B to the oil phase solution C, stirring rapidly to completely emulsify, and introducing nitrogen to deoxygenate, to obtain a thickener stock solution D;

[0039] The aqueous solution B in container A is input into container B to reduce the number of reactors used. There is no need to take the aqueous solution out of container A, and take the oily solution out of container B to mix in the third reactor.

[0040] S5: raising the temperature of the thickener stock solution D to 45 degrees Celsius to initiate the reaction, and after the reaction is completed, keeping the temperature between 40 degrees Celsius and 43 degrees Celsius for 3 hours, and then heating it to 75 degrees Celsius to react;

[0041] S6: reflux the reheated thickener stock solution D for 3 hours, and remove the solvent therein by azeotropic distillation;

[0042] S7: The dehydrated thickener stock solution D is allowed to stand until it is at room temperature, and then the emulsifier T-80 is added and stirred to gradually change phases to obtain the thickener;

[0043] The mass ratio of the emulsifier used in the phase transition of the thickener stock solution D to the oil phase solution C is 3:25 (ie, the emulsifier is 12% of the mass of the oil phase solution C).

[0044] Embodiment 2:

[0045] Based on Example 1, this example introduces the application of a thickener manufactured by a preparation process of a flexible thickener:

[0046] Experiment 1: The thickener produced by the preparation process of the flexible thickener was mixed with industrial water to obtain five white pulp samples with different concentrations (the contents of the thickener in the five white pulp samples with different concentrations were 0.1%, 0.2%, 0.4%, 0.8% and 1.0%, respectively, and the contents of the thickener in the white pulp samples were based on the application amount of the existing thickener in industrial water: 0.1% to 1%), and the viscosity of the white pulp of different samples was measured by a rotational viscometer;

[0047] In the process of measuring different samples (mixed by industrial water and thickener) by the rotational viscometer, the dosage of the thickener suitable for the application environment is determined according to the flexibility of the white pulp viscosity and the difference in viscosity between different white pulp samples;

[0048] Experiment 2: The reactive red dye was dissolved in industrial water to prepare a dye solution with a mass fraction of 0.17%, and then the dye solution was mixed with a thickener to form four color paste samples with different concentrations (the contents of thickener in the four color paste samples with different concentrations were 2%, 4%, 6% and 8%, respectively, and the content of thickener in the color paste samples was based on the existing application amount of thickener in dyes: 2% to 8%), and four color paste samples with different concentrations of thickener content were obtained, and the white slurry viscosity of different samples was measured by a rotational viscometer.

[0049] Experiment 3: Prepare Na2SO4 salt solution, and mix it with thickener to obtain three different concentrations of white pulp samples with thickener content of 3%, 4% and 5% (the content of thickener in the white pulp sample is based on the application amount of existing thickener for independent thickening in salt solution of 4%, and the measurement of thickener with deviation content is carried out according to the determined value), and the viscosity of the white pulp of different samples is measured by a rotational viscometer;

[0050] At the same time, a composite solution of Na2SO4 and active ingredients was prepared, and proportioned with a thickener to obtain eight white pulp samples of thickener with different concentrations (the contents of the thickener in the eight white pulp samples with different concentrations were 0.5%, 1%, 1.5%, 2.0%, 2.5%, 3%, 3.5 and 4%, respectively, and the content of the thickener in the white pulp samples was based on the application amount of the existing thickener in the composite solution of Na2SO4 and active ingredients: 0.5% to 4%), and the viscosity of the white pulp of different samples was measured by a rotational viscometer.

[0051] Experiment 4: Different main surfactants (sodium / ammonium lauryl sulfate, sodium / ammonium laureth sulfate and sodium α-olefin sulfonate, etc.), additives (zinc pyrithione, pyridone ethanolamine salt, ketoconazole and climbazole, etc.) and preservatives in shampoo were selected and proportioned into solutions, and then proportioned with thickeners (secondary surfactants). Four different concentrations of white pulp samples with thickener contents of 0.5%, 1.0%, 1.5% and 2.0% were prepared, and the white pulp viscosities of different samples were measured by a rotational viscometer.

[0052] Among them, referring to Experiments 1 to 4 (including but not limited to, experiments can also be conducted on printing and dyeing thickeners, etc.), referring to the viscosity of the white pulp samples with thickeners under different application environments measured by the rotational viscosity, the samples with the best flexibility under each application environment are selected and compared, and the samples with the best flexibility under different application environments are screened out. At this time, the thickener can be applied to this field to obtain a final product with better flexibility;

[0053] Specifically, the flexible thickener prepared by the above technical solution is used for thickening industrial water, independently used for thickening salt solution, thickening of solution of salt and active substance compounded, or thickening of shampoo.

[0054] Finally, it should be noted that: Obviously, the above embodiments are only examples for clearly explaining the present invention, and are not intended to limit the implementation methods. For ordinary technicians in the relevant field, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived from this are still within the scope of protection of the present invention.

Claims

1. A process for preparing a flexible thickener, characterized in that: include: Step 1: Take container A, dissolve acrylic acid monomer and methylpropane sulfonic acid monomer in water, and stir with the aid of crosslinking agent and initiator to obtain an aqueous phase mixed solvent, which is recorded as raw material solution A; Step 2: Under low temperature, add sodium hydroxide solution to the raw material solution A, and make it reach an acid-base neutralization state under the premise of monitoring the pH value of the raw material solution A by a pH monitor, which is recorded as aqueous phase solution B; Step 3: Take container B, and place a certain amount of liquid paraffin, cyclohexane, sorbitan monooleate and stabilizer therein, and stir and mix, to obtain an oil phase solution C after clarification; Step 4: Add the aqueous solution B to the oil phase solution C, stir rapidly to make it emulsified completely, and introduce nitrogen to deoxygenate, to obtain a thickener stock solution D; Step 5: Raise the temperature of thickener stock solution D to 45 degrees Celsius to initiate the reaction. After the reaction is completed, keep the temperature between 40 degrees Celsius and 43 degrees Celsius for 3 hours, and then heat it to 75 degrees Celsius to react. Step 6: reflux the reheated thickener stock solution D for 3 hours, and remove the solvent therein by azeotropic distillation; Step 7: Let the dehydrated thickener stock solution D stand until it is at room temperature, then add emulsifier T-80 and stir to gradually change phases to obtain the thickener.

2. A process for preparing a flexible thickener as claimed in claim 1, characterized in that: In the step 1, the neutralization degree of the acrylic acid monomer and the methylpropane sulfonic acid monomer is 89%-91%.

3. A process for preparing a flexible thickener as claimed in claim 1, characterized in that: The ratio of the cross-linking agent used before the raw material solution A is mixed in the step 1 to the total mass of the monomers (acrylic acid monomer and methylpropane sulfonic acid monomer) is 3:2000, and the ratio of the initiator used before the raw material solution A is mixed in the step 1 to the total mass of the monomers (acrylic acid monomer and methylpropane sulfonic acid monomer) is 1:1000.

4. A process for preparing a flexible thickener as claimed in claim 1, characterized in that: The mass ratio of the emulsifier used in the phase transition of the thickener stock solution D in step seven to the oil phase solution C is 3:

25.

5. The process for preparing a flexible thickener according to claim 1, characterized in that: The thickener obtained in step seven is mixed with industrial water to prepare five different concentrations of white pulp samples with thickener contents of 0.1%, 0.2%, 0.4%, 0.8% and 1.0%, and the viscosity of the white pulp of the different samples is measured by a rotational viscometer.

6. The process for preparing a flexible thickener according to claim 1, characterized in that: The reactive red dye is dissolved in industrial water to prepare a dye solution with a mass fraction of 0.17%, and then the dye solution is mixed with the thickener obtained in step seven to obtain four different concentrations of color paste samples with thickener contents of 2%, 4%, 6% and 8%, and the white paste viscosity of different samples is measured by a rotational viscometer.

7. The process for preparing a flexible thickener according to claim 1, characterized in that: A Na2SO4 salt solution was prepared and proportioned with the thickener obtained in step seven, and three white pulp samples with different concentrations of 3%, 4% and 5% thickener content were obtained, and the white pulp viscosities of the different samples were measured by a rotational viscometer.

8. The process for preparing a flexible thickener according to claim 1, characterized in that: A composite solution of Na2SO4 and active substances was prepared, and the solution was proportioned with the thickener obtained in step seven, and eight white slurry samples with different concentrations of thickener contents of 0.5%, 1%, 1.5%, 2.0%, 2.5%, 3%, 3.5% and 4% were obtained, and the viscosity of the white slurry of different samples was measured by a rotational viscometer.

9. The process for preparing a flexible thickener according to claim 1, characterized in that: Different main surfactants, additives and preservatives in shampoo are selected to form solutions, and are proportioned with the thickener (secondary surfactant) obtained in step seven, and four white pulp samples with different concentrations of thickener content of 0.5%, 1.0%, 1.5% and 2.0% are obtained, and the white pulp viscosity of different samples is measured by a rotational viscometer.

10. Use of the flexible thickener according to any one of claims 1 to 9 as a printing and dyeing thickener.

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