阅读说明：本技术 一种无溶剂的水性石油树脂乳液的制备方法 (Preparation method of solvent-free water-based petroleum resin emulsion ) 是由 蒋哲明 易添福 阳习春 叶武龙 刘小林 欧阳湘 王致远 周磊 于 2020-12-18 设计创作，主要内容包括：本发明提供一种无溶剂的水性石油树脂乳液的制备方法,包括以下步骤：用电子天平秤称取石油树脂和改性剂A,将石油树脂加入的反应釜中加热溶解,当反应釜中固体物完成热熔后添加改性剂A进行预处理,预处理完成后对热熔预处理后的改性石油树脂熔流体进行保温保压,取乳化剂B使用蒸馏水溶解,并持续搅拌至形成透明液体,并升高温度和压力,将保温保压的改性石油树脂熔流体和乳化剂B的水溶液泵入高压均质机中,进行乳化,高压均质机降至常温出料,制得一种无溶剂的水性石油树脂乳液,采用改性和高压均质机联机乳化工艺有效缩短水性石油树脂乳液的制备进程,工艺操作简单高效。(The invention provides a preparation method of solvent-free water-based petroleum resin emulsion, which comprises the following steps: weighing petroleum resin and a modifier A by using an electronic balance scale, adding the petroleum resin into a reaction kettle for heating and dissolving, adding the modifier A for pretreatment after solid matters in the reaction kettle are melted, carrying out heat preservation and pressure maintaining on a modified petroleum resin melt fluid after the heat preservation and pressure maintaining after the pretreatment is finished, dissolving an emulsifier B by using distilled water, continuously stirring until a transparent liquid is formed, raising the temperature and the pressure, pumping the modified petroleum resin melt fluid subjected to heat preservation and pressure maintaining and an aqueous solution of the emulsifier B into a high-pressure homogenizer for emulsification, cooling the high-pressure homogenizer to normal temperature, and discharging to prepare a solvent-free aqueous petroleum resin emulsion.)

1. A method for preparing solvent-free water-based petroleum resin emulsion is characterized in that: the method comprises the following steps: weighing the petroleum resin and the modifier A by using an electronic balance scale, and adding the petroleum resin into a reaction kettle for heating and dissolving;

step two: after the solid in the reaction kettle is subjected to hot melting, adding a modifier A for pretreatment, and after the pretreatment is finished, carrying out heat preservation and pressure maintaining on the modified petroleum resin molten fluid subjected to hot melting pretreatment;

step three: dissolving emulsifier B with distilled water, stirring to form transparent liquid, and heating to high temperature and high pressure;

step four: pumping the modified petroleum resin melt fluid with heat preservation and pressure maintaining and the water solution of the emulsifier B into a high-pressure homogenizer for emulsification;

step five: and cooling the high-pressure homogenizer to normal temperature, and discharging to obtain the solvent-free water-based petroleum resin emulsion.

2. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: in the first step, 600g of petroleum resin is weighed, the particle size of the petroleum resin D100 is 0.5-10um, and the mass of the modifier A is 10-30 g.

3. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: the heating temperature of the reaction kettle in the first step is 120-150 ℃.

4. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: and the pretreatment time in the second step is controlled to be 20-40 min.

5. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: in the second step, the molten fluid is subjected to heat preservation and pressure maintaining at the specific temperature of 60-80 ℃ and the pressure of 10-20 MPa.

6. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: the modifier A is specifically a strong electric nuclear high-temperature resistant modifier.

7. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: the weight of the emulsifier B in the third step is 10-40g, and the distilled water is 450 ml.

8. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: the emulsifier B is specifically at least one or a mixture of isomeric alcohol polyoxyethylene ether sodium sulfate compounded with sodium dodecyl diphenyl ether disulfonate, sodium tetradecyl diphenyl ether disulfonate and sodium hexadecyl diphenyl ether disulfonate.

9. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: the temperature and pressure in the third step are 80-100 ℃ and 10-20 MPa.

10. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: the emulsification temperature in the fourth step is 120-150 ℃, and the emulsification time is 1-10 min.

11. The method for preparing a solvent-free aqueous petroleum resin emulsion according to claim 1, wherein: the homogenizing pressure of the high-pressure homogenizer is 10-100MPa during emulsification in the fourth step.

Technical Field

The invention relates to the field of petroleum resin application, in particular to a preparation method of solvent-free water-based petroleum resin emulsion.

Background

Petroleum resins are a generic name for resinous materials obtained by polymerizing olefins or cycloolefins, which are by-products of cracked petroleum, or copolymerizing the same with aldehydes, aromatic hydrocarbons, terpene compounds, and the like. The petroleum resin has the characteristics of low acid value, good miscibility, low scrupulously and respectfully point, water resistance, ethanol resistance, chemical resistance and the like, is soluble in aliphatic hydrocarbon and chlorinated hydrocarbon, but is insoluble in lower alcohol and ketone. Petroleum resins are used mainly in the coatings industry, as petroleum resin emulsions are used to reinforce synthetic latex coatings, and light-colored petroleum resins are used to make oil-based varnishes for improved gloss and adhesion. Petroleum resins are also used in the rubber industry, with low softening points being used as plasticizers and higher softening points increasing the hardness of the synthetic rubber. The petroleum resin can also be used for preparing hot melt adhesive, traffic road sign paint, printing ink, paper hydrophobing agent and the like.

Petroleum resins are generally classified into four types, C5 (aliphatic), C9 (aromatic), DCPD (cyclic aliphatic diene) and pure monomer, and the constituent molecules thereof are hydrocarbons, and are also called hydrocarbon resins. The petroleum resin is also called aromatic petroleum resin, which is prepared by taking a by-product C9 fraction obtained by refining or cracking petroleum as a raw material, cutting the fraction at 140-200 ℃, wherein the content of unsaturated olefin accounts for about 40%, and the main components comprise aromatic compounds such as methyl styrene, dimethyl styrene, methyl indene, dicyclopentadiene and the like, and performing vinyl polymerization.

However, petroleum resin cannot be directly applied to a water-based system, so that the petroleum resin is usually prepared into emulsion to be applied to production, the existing preparation process of the water-based petroleum resin emulsion needs to add a large amount of solvent substances during preparation, certain influence is caused on the properties of the petroleum resin emulsion, and meanwhile, the existing preparation process of the water-based petroleum resin emulsion is complex, complicated, and high in energy consumption and material consumption.

Disclosure of Invention

Technical problem to be solved

In view of the defects of the prior art, the invention provides a preparation method of a solvent-free aqueous petroleum resin emulsion, which solves the problems in the background art.

(II) technical scheme

In order to achieve the purpose, the invention is realized by the following technical scheme: the preparation method of the solvent-free water-based petroleum resin emulsion comprises the following steps

The method comprises the following steps: weighing the petroleum resin and the modifier A by using an electronic balance scale, and adding the petroleum resin into a reaction kettle for heating and dissolving;

step two: after the solid in the reaction kettle is subjected to hot melting, adding a modifier A for pretreatment, and after the pretreatment is finished, carrying out heat preservation and pressure maintaining on the modified petroleum resin molten fluid subjected to hot melting pretreatment;

step three: dissolving emulsifier B with distilled water, stirring to form transparent liquid, and heating to high temperature and high pressure;

step four: pumping the modified petroleum resin melt fluid with heat preservation and pressure maintaining and the water solution of the emulsifier B into a high-pressure homogenizer for emulsification;

step five: and cooling the high-pressure homogenizer to normal temperature, and discharging to obtain the solvent-free water-based petroleum resin emulsion.

Preferably, 600g of petroleum resin is weighed in the first step, the particle size of the petroleum resin D100 is 0.5-10um, and the mass of the modifier A is 10-30 g.

Preferably, the heating temperature of the reaction kettle in the first step is 120-150 ℃.

Preferably, the pretreatment time in the second step is controlled to be 20-40 min.

Preferably, the temperature and pressure of the molten fluid in the second step are 60-80 ℃ and 10-20 MPa.

Preferably, the modifier A is a strong electron nuclear high-temperature resistant modifier.

Preferably, the weight of the emulsifier B in the third step is 10-40g, and the distilled water is 450 ml.

Preferably, the emulsifier B is at least one or a mixture of isomeric alcohol polyoxyethylene ether sodium sulfate compounded with sodium dodecyl diphenyl ether disulfonate, sodium tetradecyl diphenyl ether disulfonate and sodium hexadecyl diphenyl ether disulfonate.

Preferably, the temperature and pressure in the third step are increased to 80-100 ℃ and 10-20 MPa.

Preferably, the emulsification temperature in the fourth step is 120-150 ℃, and the emulsification time is 1-10 min.

Preferably, the homogenizing pressure of the high-pressure homogenizer in the emulsification in the fourth step is 10-100 MPa.

(III) advantageous effects

The invention provides a preparation method of solvent-free water-based petroleum resin emulsion, which has the following beneficial effects:

the invention adopts the modification and high-pressure homogenizer online emulsification process, solid petroleum resin is added into a closed jacket reaction kettle, the heating and melting are carried out gradually, and strong electric nuclear high-temperature resistant modifiers with different hydrophobic chain ends are added, so that the hydrophobic chain end of the modifier A and the petroleum resin are efficiently fused, the viscosity is reduced, and the polarity and the cohesion are adjusted; heating the emulsifier mixed with distilled water to the temperature of 120-150 ℃, pumping the emulsifier mixed with the petroleum resin hot-melt fluid pretreated at the front end to a high-pressure homogenizer for high-temperature high-pressure homogenizing emulsification, then cooling and depressurizing, filtering and packaging to obtain the finished product of the water-based petroleum resin emulsion.

Detailed Description

The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, such repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and/or configurations discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.

Example one

The embodiment of the invention provides a preparation method of solvent-free water-based petroleum resin emulsion, which comprises the following steps: weighing the petroleum resin and the modifier A by using an electronic balance scale, and adding the petroleum resin into a reaction kettle for heating and dissolving; step two: after the solid in the reaction kettle is subjected to hot melting, adding a modifier A for pretreatment, and after the pretreatment is finished, carrying out heat preservation and pressure maintaining on the modified petroleum resin molten fluid subjected to hot melting pretreatment;

step three: dissolving emulsifier B with distilled water, stirring to form transparent liquid, and heating to high temperature and high pressure; step four: pumping the modified petroleum resin melt fluid with heat preservation and pressure maintaining and the water solution of the emulsifier B into a high-pressure homogenizer for emulsification;

step five: and cooling the high-pressure homogenizer to normal temperature, and discharging to obtain the solvent-free water-based petroleum resin emulsion.

Wherein, in the step one, the weight of the petroleum resin is 500g, the particle size of the petroleum resin D100 is 0.5-10um, the weight of the modifier A is 20, and the heating temperature of the reaction kettle is 120 ℃.

And in the second step, the pretreatment time is controlled to be 30min, the temperature of the molten fluid is kept at 70 ℃, the pressure is 15MPa, and the modifier A is a strong electron nuclear high-temperature resistant modifier.

In the third step, the weight of the emulsifier B is 30g, the distilled water is 450ml, the emulsifier B is specifically at least one or a mixture of isomeric alcohol polyoxyethylene ether sodium sulfate compounded sodium dodecyl diphenyl ether disulfonate, sodium tetradecyl diphenyl ether disulfonate and sodium hexadecyl diphenyl ether disulfonate, and the raising temperature and the raising pressure are specifically 80 ℃ and 10 MPa.

In the fourth step, the emulsification temperature is 140 ℃, the emulsification time is 4min, and the homogenization pressure of the high-pressure homogenizer is 10-100MPa during emulsification.

The results of comparative tests conducted under homogeneous pressure of 20, 50, 70, and 90MPa are as follows

Example two

The embodiment of the invention provides a preparation method of solvent-free water-based petroleum resin emulsion, which comprises the following steps

The method comprises the following steps: weighing the petroleum resin and the modifier A by using an electronic balance scale, and adding the petroleum resin into a reaction kettle for heating and dissolving;

step two: after the solid in the reaction kettle is subjected to hot melting, adding a modifier A for pretreatment, and after the pretreatment is finished, carrying out heat preservation and pressure maintaining on the modified petroleum resin molten fluid subjected to hot melting pretreatment;

step three: dissolving emulsifier B with distilled water, stirring to form transparent liquid, and heating to high temperature and high pressure;

step four: pumping the modified petroleum resin melt fluid with heat preservation and pressure maintaining and the water solution of the emulsifier B into a high-pressure homogenizer for emulsification;

step five: and cooling the high-pressure homogenizer to normal temperature, and discharging to obtain the solvent-free water-based petroleum resin emulsion.

Wherein, in the step one, the weight of the petroleum resin is 500g, the particle size of the petroleum resin D100 is 0.5-10um, the weight of the modifier A is 20, and the heating temperature of the reaction kettle is 120 ℃.

And in the second step, the pretreatment time is controlled to be 30min, the temperature of the molten fluid is kept at 70 ℃, the pressure is 15MPa, and the modifier A is a strong electron nuclear high-temperature resistant modifier.

In the third step, the weight of the emulsifier B is 30g, the distilled water is 450ml, the emulsifier B is specifically at least one or a mixture of isomeric alcohol polyoxyethylene ether sodium sulfate compounded sodium dodecyl diphenyl ether disulfonate, sodium tetradecyl diphenyl ether disulfonate and sodium hexadecyl diphenyl ether disulfonate, and the raising temperature and the raising pressure are specifically 80 ℃ and 10 MPa.

In the fourth step, the emulsification temperature is 120-.

The emulsification temperature is 120 ℃, 130 ℃, 140 ℃ and 150 ℃ for comparison test, and the test results are shown in the table

EXAMPLE III

The embodiment of the invention provides a preparation method of solvent-free water-based petroleum resin emulsion, which comprises the following steps

The method comprises the following steps: weighing the petroleum resin and the modifier A by using an electronic balance scale, and adding the petroleum resin into a reaction kettle for heating and dissolving;

step two: after the solid in the reaction kettle is subjected to hot melting, adding a modifier A for pretreatment, and after the pretreatment is finished, carrying out heat preservation and pressure maintaining on the modified petroleum resin molten fluid subjected to hot melting pretreatment;

step three: dissolving emulsifier B with distilled water, stirring to form transparent liquid, and heating to high temperature and high pressure;

step four: pumping the modified petroleum resin melt fluid with heat preservation and pressure maintaining and the water solution of the emulsifier B into a high-pressure homogenizer for emulsification;

step five: and cooling the high-pressure homogenizer to normal temperature, and discharging to obtain the solvent-free water-based petroleum resin emulsion.

Wherein, in the step one, the weight of the petroleum resin is 500g, the particle size of the petroleum resin D100 is 0.5-10um, the weight of the modifier A is 20, and the heating temperature of the reaction kettle is 120 ℃.

And in the second step, the pretreatment time is controlled to be 30min, the temperature of the molten fluid is kept at 70 ℃, the pressure is 15MPa, and the modifier A is a strong electron nuclear high-temperature resistant modifier.

In the third step, the weight of the emulsifier B is 30g, the distilled water is 450ml, the emulsifier B is specifically at least one or a mixture of isomeric alcohol polyoxyethylene ether sodium sulfate compounded sodium dodecyl diphenyl ether disulfonate, sodium tetradecyl diphenyl ether disulfonate and sodium hexadecyl diphenyl ether disulfonate, and the raising temperature and the raising pressure are specifically 80 ℃ and 10 MPa.

In the fourth step, the emulsification temperature is 140 ℃, the emulsification time is 1-10min, and the homogenization pressure of the high-pressure homogenizer is 70MPa during emulsification.

And the emulsification time is taken to be 2 min, 4min, 6 min and 8min for comparative tests, and the test results are shown in the following table:

example four

The embodiment of the invention provides a preparation method of solvent-free water-based petroleum resin emulsion, which comprises the following steps

The method comprises the following steps: weighing the petroleum resin and the modifier A by using an electronic balance scale, and adding the petroleum resin into a reaction kettle for heating and dissolving;

step two: after the solid in the reaction kettle is subjected to hot melting, adding a modifier A for pretreatment, and after the pretreatment is finished, carrying out heat preservation and pressure maintaining on the modified petroleum resin molten fluid subjected to hot melting pretreatment;

step three: dissolving emulsifier B with distilled water, stirring to form transparent liquid, and heating to high temperature and high pressure;

step four: pumping the modified petroleum resin melt fluid with heat preservation and pressure maintaining and the water solution of the emulsifier B into a high-pressure homogenizer for emulsification;

step five: and cooling the high-pressure homogenizer to normal temperature, and discharging to obtain the solvent-free water-based petroleum resin emulsion.

Wherein, in the step one, the weight of the petroleum resin is 500g, the particle size of the petroleum resin D100 is 0.5-10um, the weight of the modifier A is 20, and the heating temperature of the reaction kettle is 120 ℃.

And in the second step, the pretreatment time is controlled to be 30min, the temperature of the molten fluid is kept at 70 ℃, the pressure is 15MPa, and the modifier A is a strong electron nuclear high-temperature resistant modifier.

In the third step, the weight of the emulsifier B is 10-40g, the distilled water is 450ml, the emulsifier B is specifically one or a mixture of isomeric alcohol polyoxyethylene ether sodium sulfate compounded with dodecyl diphenyl ether sodium disulfonate, tetradecyl diphenyl ether sodium disulfonate and hexadecyl diphenyl ether sodium disulfonate, and the rising temperature and the pressure are specifically 80 ℃ and 10 MPa.

In the fourth step, the emulsification temperature is 140 ℃, the emulsification time is 4min, and the homogenization pressure of the high-pressure homogenizer is 70MPa during emulsification.

And the emulsifier addition amount is 10, 20, 30 and 40g for comparison test, and the test results are as follows:

the experimental results show that the emulsifier is prepared by compounding sodium dodecyl diphenyl ether disulfonate with isomeric alcohol polyoxyethylene ether sulfate, the pressure is 70mpa, the emulsifying temperature is 140 ℃, the emulsifying time is 4min, and the addition of 20g of the emulsifier is the optimal emulsifying condition.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.