CN114773532B - Modified starch emulsion and preparation method thereof - Google Patents
Modified starch emulsion and preparation method thereof Download PDFInfo
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- CN114773532B CN114773532B CN202210533176.8A CN202210533176A CN114773532B CN 114773532 B CN114773532 B CN 114773532B CN 202210533176 A CN202210533176 A CN 202210533176A CN 114773532 B CN114773532 B CN 114773532B
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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Abstract
The invention belongs to the technical field of new materials, and in particular relates to an organosilicon modified starch emulsion and a preparation method thereof, wherein the organosilicon modified starch emulsion comprises the following raw materials in parts by weight: 25-35 parts of oxidized starch, 1-5 parts of inorganic catalyst, 10-15 parts of vinyl ether, 0.5-1.5 parts of peroxide initiator, 10-20 parts of comonomer, 0.5-0.6 part of preservative, 2-6 parts of stabilizer and 30-40 parts of solvent. The invention combines the advantages of acrylic ester, organic silicon and starch emulsion, ensures the film forming property, cohesiveness and shearing resistance of the emulsion, improves the heat resistance, water resistance and shearing force of the starch, has good dispersion and binding force, strong adhesive force, good emulsifying property, difficult rot and mildew and stable chemical property. And the film forming property is better than that of the original starch and the modified starch, so that a tough, continuous and uniform film can be formed, and the film has good air permeability and good adhesive force.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to an organosilicon modified starch emulsion and a preparation method thereof.
Background
Starch is a renewable natural resource, has wide sources, good cohesiveness and biodegradability and wide application range. After being denatured, the starch has new characteristics, can be used as a base material to prepare an adhesive, and is applied to various fields. The adhesive produced by using starch and its derivative as base material has good leveling property, brushing property and anti-settling property, and has the advantages of no formaldehyde and no harm to human body. And the production process is simple, the product price is low, the adhesive is an environment-friendly adhesive, and the adhesive accords with the environmental protection policy implemented by countries around the world. At present, starch derivatives mainly comprise oxidized starch and crosslinked starch, but the water resistance, mildew resistance, film strength and the like of starch-based adhesives are further improved due to the hydrophilicity and degradability of the starch. In addition, the traditional aqueous polymer adhesive such as isocyanate adhesive, urea-formaldehyde resin adhesive and the like mostly adopt synthetic resin as a main raw material, so that the adhesive has the defects of high cost, release of other harmful substances and the like. Therefore, the development of the water-based environment-friendly starch emulsion has wide market prospect.
Disclosure of Invention
The invention aims to provide an organosilicon modified starch emulsion aiming at the defects of starch in water resistance, mildew resistance, film coating strength and the like, and further improves the heat resistance, water resistance and chemical stability of starch.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the organosilicon modified starch emulsion consists of the following raw materials in parts by weight:
25-35 parts of oxidized starch, 1-5 parts of inorganic catalyst, 10-15 parts of vinyl ether, 0.5-1.5 parts of peroxide initiator, 10-20 parts of comonomer, 0.5-0.6 part of preservative, 2-6 parts of stabilizer and 30-40 parts of solvent.
Preferably, the inorganic catalyst is mercury sulfate.
Preferably, the vinyl ether is selected from one of vinyl ethyl ether, divinyl ether, vinyl diethylene glycol ether, 4-hydroxybutyl vinyl ether, 4-vinylbenzyl glycidyl ether.
Preferably, the peroxide initiator is selected from one of ammonium persulfate, potassium persulfate or sodium persulfate.
Preferably, the comonomer is selected from one of vinyl siloxane, triisopropyl silicon-based acrylate or fluorine-containing acrylate.
Preferably, the preservative is sodium benzoate.
Preferably, the stabilizer is hydroxypropyl carboxymethyl cellulose or polyvinyl alcohol.
Preferably, the solvent is selected from one of a DMSO/TBAF mixture or an ethyl acetate/TBAF mixture.
Based on one general inventive concept, another object of the present invention is to provide a method for preparing the above-mentioned silicone modified starch emulsion, comprising the steps of:
(1) Preparation of vinyl etherified starch
Uniformly mixing oxidized starch, vinyl ether and a solvent in parts by weight, dropwise adding an inorganic catalyst, heating to 40-200 ℃, refluxing, carrying out an ether exchange reaction for 2-12 h, quenching with a saturated sodium carbonate aqueous solution, extracting and separating, and removing the solvent under vacuum to obtain vinyl etherified starch;
(2) Preparation of organosilicon modified starch emulsion
Preparing vinyl etherified starch into a solution with the weight of 20-25%, adding 0.5-0.8 part of peroxide initiator, pre-initiating reaction at room temperature for 30-60 min, and regulating pH to 6.8-7.2 to obtain self-emulsifying etherified starch emulsion; then slowly adding the comonomer in parts by weight for copolymerization reaction within 30-50 min, regulating the pH to 4.5-5.5, carrying out heat preservation reaction for 1.5h at the temperature of 55-65 ℃, then adding the rest of peroxide initiator in 0-1.0 part, continuing heat preservation reaction for 1.5h at the temperature of 55-65 ℃, then adding a stabilizer and a preservative, regulating the pH to 6.8-7.2, and filtering to obtain the organosilicon modified starch emulsion.
The organosilicon modified starch emulsion prepared by the invention has uniform particle size distribution, PDI index of 0.28-0.32, emulsion particle diameter of 90-120 nm, small particle size, favorable penetration, excellent storage stability of emulsion, soaking water absorption of emulsion film approaching 0%wt, and obviously reduced surface free energy of emulsion film (from 28.1mN/m-36.5mN/m to 25.2mN/m-26.3 mN/m).
Compared with the traditional preparation method of modified starch, the preparation method of modified starch has the advantages that multiple treatments such as vinyl etherification and copolymerization are carried out on oxidized starch, the oxidized starch is adopted as a framework, etherification reaction is carried out firstly, vinyl groups are introduced, then emulsion copolymerization reaction is carried out with vinyl siloxane and silicon-containing or fluoroacrylate monomers, organosilicon groups and acrylic esters are introduced onto the starch framework, the advantages of acrylic esters, organosilicon and starch emulsion are combined, the film forming property, cohesiveness and shearing resistance of the emulsion are ensured, the heat resistance, water resistance and shearing force of starch are improved, and the modified starch has good dispersion and binding force, strong adhesive force, good emulsifying property, difficult rot and mildew and stable chemical property. And the film forming property is better than that of the original starch and the modified starch, so that a tough, continuous and uniform film can be formed, and the film has good air permeability and good adhesive force. In order to improve the crosslinking degree and stability of the emulsion, the stabilizer hydroxypropyl carboxymethyl cellulose and polyvinyl alcohol are added, and can be also complexed with hydroxyl groups in starch molecules to form hydrogen bonds to generate crosslinking, so that a polynuclear complex with a network structure is formed, the water resistance and stability of the starch emulsion are improved, the initial adhesion strength of the modified starch emulsion is improved, and the modified starch emulsion is widely applied to the fields of coating, papermaking and the like. The invention has the characteristics of simple and convenient operation, no environmental pollution, easy industrialization and the like, and can generate huge ecological environmental benefit and social economic benefit after popularization and application.
Detailed Description
The invention will be further described with reference to specific embodiments for the purpose of making the objects, technical solutions and advantages of the invention more apparent, but the invention is not limited to these examples. It should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below. In the present invention, unless otherwise specified, all parts and percentages are by mass, the equipment and materials employed, etc. are commercially available or are conventional in the art. The methods in the following examples are conventional in the art unless otherwise specified.
The terms "comprising," "including," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
Example 1
The organosilicon modified starch emulsion consists of the following raw materials in parts by weight:
30 parts of oxidized starch (carboxyl content/aldehyde content is 0.5 mol/mol), 3 parts of inorganic catalyst, 12.5 parts of vinyl ether, 1.0 part of peroxide initiator, 15 parts of comonomer, 0.55 part of preservative, 4 parts of stabilizer and 35 parts of solvent;
the inorganic catalyst is mercury sulfate, the vinyl ether is vinyl glycol ether, the peroxide initiator is ammonium persulfate, the comonomer is vinyl siloxane, and the preservative is sodium benzoate; the stabilizer is hydroxypropyl carboxymethyl cellulose, and the solvent is a DMSO/TBAF mixture.
The preparation method of the organosilicon modified starch emulsion comprises the following steps:
(1) Preparation of vinyl etherified starch
Uniformly mixing oxidized starch, vinyl ether and a solvent in parts by weight, dropwise adding an inorganic catalyst, heating to 120 ℃, refluxing, performing an ether exchange reaction for 7 hours, quenching with a saturated sodium carbonate aqueous solution, extracting and separating, and removing the solvent under vacuum to obtain vinyl etherified starch;
(2) Preparation of organosilicon modified starch emulsion
Preparing vinyl etherified starch into 22.5%wt solution, then adding 0.6 part of peroxide initiator, pre-initiating reaction at room temperature for 45min, and adjusting pH to 7.0 to obtain self-emulsifying etherified starch emulsion; then slowly adding the comonomer in parts by weight for copolymerization reaction within 40min, regulating the pH value to 5.0, carrying out heat preservation reaction for 1.5h at the temperature of 60 ℃, then adding the rest 0.4 part of peroxide initiator, continuing heat preservation reaction for 1.5h at the temperature of 60 ℃, then adding a stabilizer and a preservative, regulating the pH value to 7.0, and filtering to obtain the organosilicon modified starch emulsion.
The organosilicon modified starch emulsion film in this example had a static contact angle of 100.9 ° to deionized water, a static contact angle of 0 ° to hexadecane, a surface free energy of 25.2mN/m, and a soaking water absorption approaching 0% wt.
Example 2
The organosilicon modified starch emulsion consists of the following raw materials in parts by weight:
35 parts of oxidized starch (carboxyl content/aldehyde content is 0.6 mol/mol), 1 part of inorganic catalyst, 15 parts of vinyl ether, 0.5 part of peroxide initiator, 20 parts of comonomer, 0.5 part of preservative, 6 parts of stabilizer and 30 parts of solvent;
the inorganic catalyst is mercury sulfate, the vinyl ether is vinyl diethyl ether, the peroxide initiator is potassium persulfate, the comonomer is triisopropyl silicon-based acrylate, the preservative is sodium benzoate, the stabilizer is 1799 type polyvinyl alcohol (the polymerization degree is 1700, the hydrolysis degree is 88% -99%), and the solvent is ethyl acetate/TBAF mixture.
The preparation method of the organosilicon modified starch emulsion comprises the following steps:
(1) Preparation of vinyl etherified starch
Uniformly mixing oxidized starch, vinyl ether and a solvent in parts by weight, dropwise adding an inorganic catalyst, heating to 180 ℃, refluxing, carrying out an ether exchange reaction for 4 hours, quenching with a saturated sodium carbonate aqueous solution, extracting and separating, and removing the solvent under vacuum to obtain vinyl etherified starch;
(2) Preparation of organosilicon modified starch emulsion
Preparing vinyl etherified starch into 25%wt solution, then adding 0.5 part of peroxide initiator, pre-initiating reaction at room temperature for 60min, and adjusting pH to 6.8 to obtain self-emulsifying etherified starch emulsion; then slowly adding the comonomer in parts by weight for copolymerization reaction within 50min, regulating the pH value to 4.5, carrying out heat preservation reaction for 1.5h at the temperature of 65 ℃, then adding the rest 0.5 part of peroxide initiator, continuing heat preservation reaction for 1.5h at the temperature of 65 ℃, then adding a stabilizer and a preservative, regulating the pH value to 6.8, and filtering to obtain the organosilicon modified starch emulsion.
The organosilicon modified starch emulsion film in this example had a static contact angle of 100.8 ° to deionized water, a static contact angle of 0 ° to hexadecane, a surface free energy of 25.9mN/m, and a soaking water absorption approaching 0% wt.
Example 3
The organosilicon modified starch emulsion consists of the following raw materials in parts by weight:
25 parts of oxidized starch (carboxyl content/aldehyde content is 0.4 mol/mol), 5 parts of inorganic catalyst, 10 parts of vinyl ether, 1.5 parts of peroxide initiator, 10 parts of comonomer, 0.6 part of preservative, 2 parts of stabilizer and 40 parts of solvent.
The inorganic catalyst is mercury sulfate, the vinyl ether is 4-vinylbenzyl glycidyl ether, the peroxide initiator is sodium persulfate, the comonomer is fluorine-containing acrylic ester, the preservative is sodium benzoate, the stabilizer is 1788 type polyvinyl alcohol (the polymerization degree is 1700, the hydrolysis degree is 88% -99%), and the solvent is DMSO/TBAF mixture.
The preparation method of the organosilicon modified starch emulsion comprises the following steps:
(1) Preparation of vinyl etherified starch
Uniformly mixing oxidized starch, vinyl ether and a solvent in parts by weight, dropwise adding an inorganic catalyst, heating to 50 ℃, refluxing, carrying out an ether exchange reaction for 12 hours, quenching with a saturated sodium carbonate aqueous solution, extracting and separating, and removing the solvent under vacuum to obtain vinyl etherified starch;
(2) Preparation of organosilicon modified starch emulsion
Preparing vinyl etherified starch into a solution with 20%wt, adding 0.8 part of peroxide initiator, pre-initiating reaction at room temperature for 30min, and adjusting pH to 7.2 to obtain self-emulsifying etherified starch emulsion; then slowly adding the comonomer in parts by weight for copolymerization reaction within 30min, regulating the pH to 5.5, carrying out heat preservation reaction for 1.5h at the temperature of 55 ℃, then adding the rest 0.2 part of peroxide initiator, continuing heat preservation reaction for 1.5h at the temperature of 55 ℃, then adding a stabilizer and a preservative, regulating the pH to 7.2, and filtering to obtain the organosilicon modified starch emulsion.
The organosilicon modified starch emulsion film in this example had a static contact angle of 100.7 ° to deionized water, a static contact angle of 0 ° to hexadecane, a surface free energy of 26.3mN/m, and a soaking water absorption approaching 0% wt.
Comparative example 1
Starch having an oxidation degree (carboxyl group content/aldehyde group content) of 0.3mol/mol was selected as a raw material, and the same as in example 1 was repeated.
The organosilicon modified starch emulsion film in this comparative example had a static contact angle of 60.2 ° to deionized water, a static contact angle of 0.2 ° to hexadecane, a surface free energy of 38.6mN/m, and a soaking water absorption approaching 0.5% wt.
Comparative example 2
Starch having an oxidation degree (carboxyl group content/aldehyde group content) of 0.6mol/mol was selected as a raw material, and the same as in example 1 was repeated.
The organosilicon modified starch emulsion film in this comparative example had a static contact angle of 58.6 ° to deionized water, a static contact angle of 0.1 ° to hexadecane, a surface free energy of 36.9mN/m, and a soaking water absorption approaching 0.2% wt.
Comparative example 3
The inorganic catalyst was not contained, and the other was the same as in example 1.
The organosilicon modified starch emulsion film in this comparative example had a static contact angle of 62.8 ° to deionized water, a static contact angle of 0.1 ° to hexadecane, a surface free energy of 39.1mN/m, and a soaking water absorption approaching 0.3% wt.
Comparative example 4
The component hydroxypropyl carboxymethyl cellulose was not contained, and the other was the same as in example 1.
The organosilicon modified starch emulsion film in this comparative example had a static contact angle of 58.4 ° to deionized water, a static contact angle of 0.1 ° to hexadecane, a surface free energy of 38.9mN/m, and a soaking water absorption approaching 0.1% wt.
Comparative example 5
Component 1788 type polyvinyl alcohol was not contained, and the other was the same as in example 1.
The organosilicon modified starch emulsion film in this comparative example had a static contact angle of 59.2 ° to deionized water, a static contact angle of 0.1 ° to hexadecane, a surface free energy of 37.3mN/m, and a soaking water absorption approaching 0.1% wt.
Comparative example 6
The components hydroxypropyl carboxymethyl cellulose and 1788 type polyvinyl alcohol were not contained, and the other components were the same as in example 1.
The organosilicon modified starch emulsion film in this comparative example had a static contact angle of 56.3 ° to deionized water, a static contact angle of 0.2 ° to hexadecane, a surface free energy of 39.8mN/m, and a soaking water absorption approaching 0.3% wt.
Comparative example 7
Oxidized starch prepared by nitric acid oxidation is adopted, starch with the oxidation degree (carboxyl content/aldehyde content) of 0.4mol/mol is selected as a raw material, 40% of oxidized starch milk and 20% of polyvinyl alcohol solution are respectively added into a 500ml four-neck flask provided with a stirrer and a thermometer, the weight ratio of the oxidized starch to the polyvinyl alcohol in the solution is 0.2, 10% of hydrochloric acid is added to adjust the pH=2.5 of the solution, and the solution is heated to 65 ℃ for crosslinking reaction for 2 hours. Adding vinyl trimethoxy siloxane monomer accounting for 4% of the weight of the polyvinyl alcohol, stirring uniformly for 30 minutes, then dripping 3% potassium persulfate solution to initiate reaction, and reacting for 5 hours at the temperature of 60-80 ℃ to obtain the organosilicon modified oxidized starch emulsion.
The organosilicon modified starch emulsion film in this comparative example had a static contact angle of 60.9 ° to deionized water, a static contact angle of 0.1 ° to hexadecane, a surface free energy of 38.2mN/m, and a soaking water absorption approaching 0.1% wt.
Test example 1
The silicone modified starch emulsions prepared in examples 1 to 3 and comparative examples 1 to 7 were subjected to performance tests with reference to GB/T9755-2001 synthetic resin emulsion exterior wall coating standards, and the water resistance and alkali resistance indexes thereof were tested according to GB/T1733 and GB/T9265, and the performance was measured according to the standards as shown in Table 1 below.
TABLE 1 results of Performance measurements for examples 1-3 and comparative examples 1-7
The above embodiments are merely preferred embodiments of the present invention, and any simple modification, modification and substitution changes made to the above embodiments according to the technical substance of the present invention are all within the scope of the technical solution of the present invention.
Claims (6)
1. The modified starch emulsion is characterized by comprising the following raw materials in parts by weight:
25-35 parts of oxidized starch, 1-5 parts of mercuric sulfate, 10-15 parts of vinyl ether, 0.5-1.5 parts of peroxide initiator, 10-20 parts of comonomer, 0.5-0.6 part of preservative, 2-6 parts of stabilizer and 30-40 parts of solvent; wherein the comonomer is selected from one of vinyl siloxane, triisopropyl silicon-based acrylate or fluorine-containing acrylate, and the stabilizer is hydroxypropyl carboxymethyl cellulose or polyvinyl alcohol;
the preparation method of the modified starch emulsion comprises the following steps:
(1) Preparation of vinyl etherified starch
Uniformly mixing oxidized starch, vinyl ether and a solvent in parts by weight, dropwise adding mercuric sulfate, heating to 40-200 ℃, refluxing, performing an ether exchange reaction for 2-12 h, quenching with a saturated sodium carbonate aqueous solution, extracting and separating, and removing the solvent under vacuum to obtain vinyl etherified starch;
(2) Preparation of modified starch emulsion
Preparing vinyl etherified starch into a solution with the weight of 20-25%, adding 0.5-0.8 part of peroxide initiator, pre-initiating reaction at room temperature for 30-60 min, and regulating pH to 6.8-7.2 to obtain self-emulsifying etherified starch emulsion; then slowly adding the comonomer in parts by weight for copolymerization reaction within 30-50 min, regulating the pH to 4.5-5.5, carrying out heat preservation reaction for 1.5h at the temperature of 55-65 ℃, then adding the rest of peroxide initiator in 0-1.0 part, continuing heat preservation reaction for 1.5h at the temperature of 55-65 ℃, then adding a stabilizer and a preservative, regulating the pH to 6.8-7.2, and filtering to obtain the modified starch emulsion.
2. A modified starch emulsion according to claim 1 wherein said vinyl ether is selected from one of vinyl ethyl ether, divinyl ether, vinyl diethylene glycol ether, 4-hydroxybutyl vinyl ether, 4-vinylbenzyl glycidyl ether.
3. A modified starch emulsion according to claim 1, wherein the peroxide initiator is selected from one of ammonium persulfate, potassium persulfate or sodium persulfate.
4. The modified starch emulsion of claim 1, wherein the preservative is sodium benzoate.
5. A modified starch emulsion according to claim 1, wherein the solvent is selected from one of DMSO/TBAF mixture or ethyl acetate/TBAF mixture.
6. A method for preparing a modified starch emulsion as claimed in any one of claims 1 to 5, comprising the steps of:
(1) Preparation of vinyl etherified starch
Uniformly mixing oxidized starch, vinyl ether and a solvent in parts by weight, dropwise adding mercuric sulfate, heating to 40-200 ℃, refluxing, performing an ether exchange reaction for 2-12 h, quenching with a saturated sodium carbonate aqueous solution, extracting and separating, and removing the solvent under vacuum to obtain vinyl etherified starch;
(2) Preparation of modified starch emulsion
Preparing vinyl etherified starch into a solution with the weight of 20-25%, adding 0.5-0.8 part of peroxide initiator, pre-initiating reaction at room temperature for 30-60 min, and regulating pH to 6.8-7.2 to obtain self-emulsifying etherified starch emulsion; then slowly adding the comonomer in parts by weight for copolymerization reaction within 30-50 min, regulating the pH to 4.5-5.5, carrying out heat preservation reaction for 1.5h at the temperature of 55-65 ℃, then adding the rest of peroxide initiator in 0-1.0 part, continuing heat preservation reaction for 1.5h at the temperature of 55-65 ℃, then adding a stabilizer and a preservative, regulating the pH to 6.8-7.2, and filtering to obtain the modified starch emulsion.
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