阅读说明：本技术 一种缸中硅油及其制备方法 (In-cylinder silicone oil and preparation method thereof ) 是由 沈建亮 张桃勇 张金龙 于 2020-12-28 设计创作，主要内容包括：本申请涉及纺织助剂的技术领域,具体公开了一种缸中硅油及其制备方法,缸中硅油,由包括以下质量百分比的原料制备得到：哌嗪基聚醚改性硅油5%～20%；复合乳化剂0.5%～2.5%；冰醋酸0.05%～0.5%；抗凝聚剂3%～10%；去离子水余量；其制备方法为：步骤1：将哌嗪基聚醚改性硅油和复合乳化剂混合并进行搅拌,搅拌时间为25-35min,得中间物A；步骤2：将冰醋酸和部分去离子水混合物,加入到中间物A中,搅拌25-35min,得中间物B；步骤3：将剩余的去离子水匀速滴加到中间物B中,滴加时间为110-130min,滴加完成后得到中间物C；步骤4：将抗凝聚剂加入到中间物C中,搅拌8-12min,即得到缸中硅油；本申请的缸中硅油具有不易破乳、漂油,易于同浴进缸使用的效果。(The application relates to the technical field of textile auxiliary agents, and particularly discloses silicone oil in a cylinder and a preparation method thereof, wherein the silicone oil in the cylinder is prepared from the following raw materials in percentage by mass: 5-20% of piperazinyl polyether modified silicone oil; 0.5 to 2.5 percent of composite emulsifier; glacial acetic acid 0.05% -0.5%; 3 to 10 percent of anti-agglomeration agent; the balance of deionized water; the preparation method comprises the following steps: step 1: mixing the piperazinyl polyether modified silicone oil and the composite emulsifier, and stirring for 25-35min to obtain an intermediate A; step 2: adding a mixture of glacial acetic acid and part of deionized water into the intermediate A, and stirring for 25-35min to obtain an intermediate B; and step 3: dropwise adding the rest deionized water into the intermediate B at a constant speed for 110-; and 4, step 4: adding the anti-agglomeration agent into the intermediate C, and stirring for 8-12min to obtain silicone oil in the cylinder; the silicone oil in the cylinder has the effects of difficult demulsification and oil floating and easy use in one bath.)

1. Silicon oil in a cylinder is characterized in that: the material is prepared from the following raw materials in percentage by mass:

2. silicone oil in a cylinder according to claim 1, characterized in that: the piperazinyl polyether modified silicone oil is prepared from the following components in percentage by mass:

3. silicone oil in a cylinder according to claim 2, characterized in that: the structural general formula of the hydrogen-terminated silicone oil is as follows:

wherein m is an integer of 60-200, and the average molecular weight is 4500-14860.

4. Silicone oil in a cylinder according to claim 2, characterized in that: the general structural formula of the allyl epoxy polyether is as follows:

wherein x is an integer of 4-20; y is an integer of 4 to 20, and the average molecular weight is 508 to 2140.

5. Silicone oil in a cylinder according to claim 2, characterized in that: the piperazinyl compound is one or more of gamma-piperazinyl propyl methyl dimethoxysilane, N-methylpiperazine, N-ethylpiperazine, 1-isopropylpiperazine, 1-cyclohexylpiperazine and 1-tert-butyloxycarbonylpiperazine.

6. Silicone oil in a cylinder according to any one of claims 2-5, characterised in that: the preparation process of the piperazinyl polyether modified silicone oil comprises the following steps:

s1: mixing and uniformly stirring hydrogen-terminated silicone oil and allyl epoxy polyether according to the mass ratio, heating to 60-75 ℃, starting reflux condensation, adding a mixture of chloroplatinic acid and isopropanol, continuously heating to 80-85 ℃, and carrying out heat preservation reaction for 3 hours to obtain the M-type epoxy-terminated polyether silicone oil;

s2: adding a mixture of a piperazinyl compound and isopropanol into the epoxy terminated polyether silicone oil of the formula M, and continuously reacting for 5 hours at a constant temperature to obtain piperazinyl polyether modified silicone oil; the reaction formula is as follows:

wherein R1 is one of methyl, ethyl, isopropyl, cyclohexyl, tert-butyloxycarbonyl or propyl-methyldimethoxysilane.

7. Silicone oil in a cylinder according to any one of claims 1-5, characterised in that: the composite emulsifier is obtained by mixing a main emulsifier and an auxiliary emulsifier according to the mass percentage of 3:1, wherein the main emulsifier is a polyether organic silicon surfactant, and the structural general formula of the polyether organic silicon surfactant is as follows:

wherein n is an integer of 10 to 20, and the average molecular weight is 1680 to 2560.

8. Silicone oil in a cylinder according to claim 7, characterised in that: the auxiliary emulsifier is one or more of alcohol ether carboxylic acid, oleyl alcohol polyoxyethylene ether, cardanol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, heterogeneous alcohol polyoxyethylene ether and castor oil polyoxyethylene ether.

9. Silicone oil in a cylinder according to any one of claims 1-5, characterised in that: the anti-condensation agent is fatty alcohol-polyoxyethylene ether silane, and the structural general formula of the fatty alcohol-polyoxyethylene ether silane is as follows:

wherein R2 is C12-C18 alkyl, and the average molecular weight is 3850-4102.

10. A method for preparing silicone oil in a cylinder according to any one of claims 1 to 9, characterized in that: the method comprises the following steps:

step 1: mixing the piperazinyl polyether modified silicone oil and the composite emulsifier, and stirring for 25-35min to obtain an intermediate A;

step 2: adding a mixture of glacial acetic acid and part of deionized water into the intermediate A, and stirring for 25-35min to obtain an intermediate B;

and step 3: dropwise adding the rest deionized water into the intermediate B at a constant speed for 110-;

and 4, step 4: and adding the anti-agglomeration agent into the intermediate C, and stirring for 8-12min to obtain the silicone oil in the cylinder.

Technical Field

The application relates to the field of textile auxiliary agents, in particular to silicone oil in a cylinder and a preparation method thereof.

Background

The organic silicon softening agent has the characteristics of softness, smoothness, fluffiness, stiffness, elasticity, hydrophilicity and the like of the fabric, so that the organic silicon softening agent is widely applied to the after-finishing processing of the fabric.

However, with the diversification of fabric types, the complication of processing technology, cost saving and energy saving and emission reduction requirements, the printing and dyeing mill is expected to develop a silicone oil softener which can be used in one bath with pretreatment and dyeing auxiliaries besides pursuing the hand feeling style of fabric differentiation. Therefore, the production process can be shortened, the working efficiency is improved, the sewage discharge is reduced, and the effects of saving cost, saving energy and reducing emission are achieved.

In view of the above-mentioned related technologies, the inventors believe that since a large amount of anionic additives, electrolytes, acid and alkali substances must be added during the pretreatment or dyeing of the fabric, and the processing process is generally carried out at high temperature, if the conventional silicone oil is used in a jar in one bath, the conventional silicone oil has poor stability in such an environment, and often breaks emulsion, floats oil, and forms oil spots on the fabric.

Disclosure of Invention

In order to solve the problem that the conventional silicone oil is difficult to enter a cylinder for one-bath use in the textile printing and dyeing process, the application provides the silicone oil in the cylinder and a preparation method thereof.

In a first aspect, the present application provides a silicone oil in a cylinder, which adopts the following technical scheme:

the silicone oil in the cylinder is prepared from the following raw materials in percentage by mass:

by adopting the technical scheme, the composition and the proportion of the silicone oil in the cylinder are specially limited, and the piperazinyl polyether modified silicone oil is specially added, so that the molecular chain of the silicone oil in the prepared cylinder has a piperazine structure and a polyether group. Because the molecular chain of the silicone oil contains piperazine structure and polyether group, the finished fabric has the characteristics of small yellowing, hydrophilicity, soft and smooth hand feeling and the like. The piperazinyl polyether modified silicone oil also has a certain self-emulsifying effect due to the characteristics of groups, so that the possibility of demulsification is reduced.

The addition amount of glacial acetic acid is controlled, and positive charges on amino groups of a silicone oil chain segment are reduced, so that the cationic property of the silicone oil is controlled, and the stability of the silicone oil in an anionic auxiliary agent is improved; the silicone oil can be effectively coated by adding the anti-coagulation agent, and various external additives, electrolytes and the like can be prevented from damaging the stability of the silicone oil, so that the whole silicone oil emulsion forms a stable system.

Namely, the prepared silicone oil in the cylinder has high stability and better tolerance to high temperature, electrolyte and acid and alkali by selecting the specific piperazinyl polyether modified silicone oil, combining the emulsification, dispersion and blocking effects of the composite emulsifier and the anti-coagulation agent and the charge influence effect of glacial acetic acid and realizing the synergistic interaction of multiple components, and the possibility of demulsification and oil floating of the silicone oil when the silicone oil is used in one bath in the cylinder is reduced.

Optionally, the piperazinyl polyether modified silicone oil is prepared from the following components in percentage by mass:

by adopting the technical scheme, the raw material components and the proportion of the piperazinyl polyether modified silicone oil are specifically limited, in the preparation process, a piperazine structure is introduced into a molecular chain of the piperazinyl polyether modified silicone oil, the piperazinyl contains a secondary amine group and a tertiary amine group, a hydrogen atom on the secondary amine group is replaced by an epoxy bond, the secondary amine group is changed into a tertiary amine group, the hydrophilicity of the silicone oil is improved, and the tertiary amine group is relatively stable and is not easy to be oxidized to cause yellowing.

In addition, a polyether group is embedded in a silicone oil molecular chain, and a polyoxyethylene ether structure and a polyoxypropylene ether structure in the polyether group provide hydrophilicity for the whole silicone oil chain segment, improve the hydrophilicity and the stability of the silicone oil structure, and greatly reduce the phenomenon of demulsification and oil floating of common silicone emulsion in the using process. In addition, the dosage of the chloroplatinic acid must be strictly controlled, because if the dosage of the chloroplatinic acid is too small, the reaction is insufficient, and the hand feeling is influenced; if the dosage of the chloroplatinic acid is too large, the problem that the silicone oil is easy to yellow after storage is easy to occur.

Optionally, the structural general formula of the hydrogen-terminated silicone oil is:

wherein m is an integer of 60-200, and the average molecular weight is 4500-14860.

By adopting the technical scheme, the molecular weight range of the finally prepared piperazinyl polyether modified silicone oil is determined by the selection of the hydrogen-terminated silicone oil, and the molecular weight of the piperazinyl polyether modified silicone oil greatly influences the quality of the silicone oil in the cylinder. If the molecular weight of the piperazinyl polyether modified silicone oil is too high, the fabric treated by the silicone oil in the cylinder is hard to handle and has poor wearability; if the molecular weight of the piperazinyl polyether modified silicone oil is too low, the fabric treated by the silicone oil in the cylinder often cannot achieve the required soft hand feeling, so that the selection of the hydrogen-containing silicone oil is very important. Through a large number of experiments of the inventor, the prepared cylinder silicone oil has the optimal performance when the average molecular weight of the hydrogen-containing silicone oil at the limited end is 4500-14860. The silicone oil prepared by limiting the average molecular weight of the end hydrogen-containing silicone oil not only reduces the possibility of poor hand feeling of the fabric caused by too small molecular weight, but also reduces the probability of dead hand feeling of the fabric caused by too large molecular weight, and the silicone oil prepared by specially selecting the end hydrogen-containing silicone oil in the molecular weight range has soft and smooth hand feeling.

Optionally, the general structural formula of the allyl epoxy polyether is:

wherein x is an integer of 4-20; y is an integer of 4 to 20, and the average molecular weight is 508 to 2140.

By adopting the technical scheme, the piperazinyl polyether modified silicone oil has certain self-emulsibility, but the piperazinyl polyether modified silicone oil does not necessarily show hydrophilicity, because the length of the lipophilic chain segment of the piperazinyl polyether modified silicone oil is longer and stronger lipophilicity is shown. In order for the piperazinyl polyether modified silicone oil to exhibit sufficient, but not excessive, hydrophilicity, the molecular weight of the allyl epoxy polyether must be very strictly controlled.

The reason is that when the hydrophilicity of the piperazinyl polyether modified silicone oil is insufficient, the silicone oil in the prepared cylinder is easy to have the problems of demulsification, oil floating and the like; when the hydrophilicity of the piperazinyl polyether modified silicone oil is too strong, the performance of the prepared silicone oil in the cylinder is closer to that of water-based silicone oil, and the hand feeling of the treated fabric is poor. Therefore, the ratio of the lipophilic chain segment and the hydrophilic chain segment in the piperazinyl polyether modified silicone oil must be comprehensively considered so as to obtain the silicone oil with both stability and hand feeling in the cylinder.

The inventor unexpectedly finds that the silicone oil in the cylinder with good stability and hand feeling is obtained when the average molecular weight of the hydrogen-containing silicone oil at the control end is 4500-14860 and the average molecular weight of the allyl epoxy polyether is 508-2140 through controlling the molecular weights of the hydrogen-containing silicone oil at the control end and the allyl epoxy polyether.

Optionally, the piperazinyl compound is one or more of gamma-piperazinylpropylmethyldimethoxysilane, N-methylpiperazine, N-ethylpiperazine, 1-isopropylpiperazine, 1-cyclohexylpiperazine and 1-tert-butoxycarbonylpiperazine.

By adopting the technical scheme, when the terminal hydrogen-containing silicone oil reacts with the allyl epoxy polyether, alkenyl on the allyl epoxy polyether reacts with active terminated hydrogen of the terminal hydrogen-containing silicone oil, and one side of epoxy on the allyl epoxy polyether reacts with the piperazinyl compound to form hydroxyl with reaction activity, and the hydroxyl with reaction activity can form chemical crosslinking with fabric, so that the fixing force of the silicone oil on the fabric in a cylinder is greatly improved, and the fastness to washing of the silicone oil is improved. Meanwhile, due to the special structure of the piperazinyl group, a shielding effect is generated on the cationic property of the tertiary amino group, the compatibility of the silicone oil and an anionic auxiliary agent in the cylinder is facilitated, and the possibility of demulsification and oil floating when the silicone oil in the cylinder enters the cylinder for use is further reduced.

Optionally, the preparation process of the piperazinyl polyether modified silicone oil comprises the following steps:

s1: mixing and uniformly stirring hydrogen-terminated silicone oil and allyl epoxy polyether according to the mass ratio, heating to 60-75 ℃, starting reflux condensation, adding a mixture of chloroplatinic acid and isopropanol, continuously heating to 80-85 ℃, and carrying out heat preservation reaction for 3 hours to obtain the M-type epoxy-terminated polyether silicone oil;

s2: adding a mixture of a piperazinyl compound and isopropanol into the epoxy terminated polyether silicone oil of the formula M, and continuously reacting for 5 hours at a constant temperature to obtain piperazinyl polyether modified silicone oil; the reaction formula is as follows:

wherein R1 is methyl, ethyl, isopropyl, cyclohexyl, tert-butyloxycarbonyl or propylmethyldimethoxysilane.

By adopting the technical scheme, the specific terminal hydrogen-containing silicone oil and the allyl epoxy polyether are selected, the terminal epoxy polyether silicone oil is prepared through the silicon hydrogen reaction, and then the piperazinyl polyether modified silicone oil with balanced hydrophilicity and lipophilicity is prepared through the reaction of the terminal epoxy polyether silicone oil and the piperazinyl compound.

The hydrosilation reaction in the step S1 is an exothermic reaction, and if the reaction temperature is too high, the reaction speed is increased too fast, the reaction process is difficult to control, which easily causes ring opening of the epoxy group that does not participate in the reaction, and affects the proceeding of the step S2. If the reaction temperature is too low, although the reaction is exothermic and the reaction process is accelerated, the basic speed is low and the final reaction time is still too long. The inventor finds that the reaction temperature is controlled to be 80-85 ℃, and the reaction end point can be reached in a relatively short reaction time, namely 3 hours, on the premise of reducing the damage to epoxy groups.

Optionally, the composite emulsifier is obtained by mixing a main emulsifier and an auxiliary emulsifier according to a mass ratio of 3:1, wherein the main emulsifier is a polyether organic silicon surfactant, and the structural general formula of the polyether organic silicon surfactant is as follows:

wherein n is an integer of 10 to 20, and the average molecular weight is 1680 to 2560.

By adopting the technical scheme, the molecular chain of the polyether organic silicon surfactant contains the organic silicon chain segment similar to the piperazinyl polyether modified silicone oil, so that the polyether organic silicon surfactant can be well distributed on the surface of the silicone oil to form a compact protective layer, and a stable silicone oil emulsion system is formed by combining the coating effect of the auxiliary emulsifier. Meanwhile, as the molecules of the polyether organic silicon surfactant contain a large number of polyoxyethylene chain segments, a layer of hydrophilic film can be formed on the surface of the fabric, so that the hydrophilicity of the finished fabric is improved.

Optionally, the auxiliary emulsifier is one or more of alcohol ether carboxylic acid, oleyl alcohol polyoxyethylene ether, cardanol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, heterogeneous alcohol polyoxyethylene ether and castor oil polyoxyethylene ether.

By adopting the technical scheme, the wetting, penetrating and emulsifying coating effects of the auxiliary emulsifier are utilized to achieve the synergistic interaction with the main emulsifier, so that a stable silicone oil emulsion system is formed.

Optionally, the anti-coagulation agent is fatty alcohol-polyoxyethylene ether silane, and the structural general formula of the fatty alcohol-polyoxyethylene ether silane is as follows:

wherein R2 is C12-C18 alkyl, and the average molecular weight is 3850-4102.

By adopting the technical scheme, the fatty alcohol-polyoxyethylene ether silane can be tightly adsorbed on the surface of the silicone oil according to the principle of similar compatibility because the fatty alcohol-polyoxyethylene ether silane contains silicon atoms, so that the silicone oil emulsion forms a stable system. Meanwhile, as the molecular weight is larger and the dispersibility is good, a better barrier effect can be formed between the silicone oil and the anionic assistant, the influence of various assistants in the pre-finishing process can be greatly reduced, the possibility of aggregation of the silicone oil is reduced, and the possibility of silicone oil stain formation on the fabric due to the fact that the silicone oil is stained is also reduced.

In a second aspect, the present application provides a method for preparing silicone oil in a cylinder, using the following technical scheme:

a preparation method of silicone oil in a cylinder comprises the following steps:

step 1: mixing the piperazinyl polyether modified silicone oil and the composite emulsifier, and stirring for 25-35min to obtain an intermediate A;

step 2: adding a mixture of glacial acetic acid and part of deionized water into the intermediate A, and stirring for 25-35min to obtain an intermediate B;

and step 3: dropwise adding the rest deionized water into the intermediate B at a constant speed for 110-;

and 4, step 4: and adding the anti-agglomeration agent into the intermediate C, and stirring for 8-12min to obtain the silicone oil in the cylinder.

By adopting the technical scheme, the composite emulsifier and the piperazinyl polyether modified silicone oil are fully mixed, so that the silicone oil chain segment is coated by enough emulsifier, and the emulsion with uniform particle size is favorably finally obtained; adding a mixture of glacial acetic acid and water to cationize amino on silicone oil molecules to form weak positive charge repulsion, reducing silicone oil chain segment aggregation in the emulsification process to form emulsion particles with different particle sizes, and gradually converting the emulsion from water-in-oil to oil-in-water state with the gradual addition of deionized water until the emulsion particles can be mixed with water; and finally, adding an anti-coagulation agent, and forming a good barrier effect between the silicone oil and other auxiliaries by utilizing the characteristics of similar structure, larger molecular weight and good dispersibility of the anti-coagulation agent and the silicone oil to form a stable emulsion system, so that the possibility that the silicone oil demulsification floating oil is stained on the fabric to form silicone oil spots is reduced.

In summary, the present application includes at least one of the following beneficial technical effects:

1. by limiting the composition and the proportion of the silicon oil raw material in the cylinder, and specifically adding the piperazinyl polyether modified silicon oil to be matched with the composite emulsifier and the glacial acetic acid, the silicon oil can be better wrapped, and the possibility of demulsification and oil floating when the silicon oil is used in one bath in the cylinder is greatly reduced;

2. by limiting the composition and proportion of the piperazinyl silicone oil raw material, the hydrophilicity and the washing resistance of the silicone oil in the cylinder can be improved, and the possibility of oxidative yellowing of the silicone oil is reduced;

3. the average molecular weight of hydrogen-containing silicone oil at the opposite end is limited, and the average molecular weight of allyl epoxy polyether is limited, so that silicone oil in a cylinder with a reasonable proportion of oleophylic chain segments and hydrophilic chain segments and good stability and hand feeling is obtained;

4. the specific preparation method is selected through the specific formula of the silicone oil in the cylinder, so that the silicone oil in the cylinder which is difficult to demulsify and float can be better prepared.

Drawings

FIG. 1 is a flow chart of a preparation process of piperazinyl polyether modified silicone oil in a preparation example of the application.

FIG. 2 is a flow chart of a preparation process of silicone oil in a cylinder according to an embodiment of the present application.

Detailed Description

The present application is described in further detail below with reference to figures 1-2.

The raw materials used in the present application are all conventionally commercially available except where indicated.

Preparation example

Preparation example 1 of Piperazinylpolyether-modified Silicone oil

The piperazinyl polyether modified silicone oil is prepared from the following components in percentage by mass:

the structural general formula of the hydrogen-terminated silicone oil is as follows:

m is an integer of 60-200, and the average molecular weight of the terminal hydrogen-containing silicone oil is 5166.

The general structural formula of the allyl epoxy polyether is as follows:

x is an integer of 4-20; y is an integer of 4-20; and the average molecular weight of the allyl epoxy polyether is 610.

The piperazinyl compound is gamma-piperazinylpropylmethyldimethoxysilane and is available from Hubei Ferry chemical Co.

Referring to fig. 1, the preparation method of the piperazinyl polyether modified silicone oil specifically comprises the following process steps:

s1: according to the mass ratio, mixing and uniformly stirring the hydrogen-terminated silicone oil and the allyl epoxy polyether, heating to 70 ℃, starting reflux condensation, adding a mixture of chloroplatinic acid and isopropanol, continuing heating to 80 ℃, and carrying out heat preservation reaction for 3 hours to obtain the M-type epoxy polyether silicone oil. The reaction formula is as follows:

s2: and adding a mixture of gamma-piperazinylpropylmethyldimethoxysilane and isopropanol into the epoxy polyether silicone oil with the formula M, and continuously reacting for 5 hours under the condition of heat preservation to obtain the piperazinylpolyether modified silicone oil. The reaction formula is as follows:

wherein R1 has a structural formula

Preparation examples 2 to 6 of piperazinyl polyether modified silicone oil are distinguished from preparation example 1 of piperazinyl polyether modified silicone oil by the following table:

among them, N-methylpiperazine, N-ethylpiperazine, 1-isopropylpiperazine, 1-cyclohexylpiperazine and 1-tert-butoxycarbonylpiperazine were purchased from Hubei Ferry chemical Co., Ltd.

Examples

The present application is described in further detail below with reference to fig. 2.

The embodiment of the application discloses in-cylinder silicone oil and a preparation method thereof.

Example 1

The silicon oil in the cylinder is prepared from the following raw materials in percentage by mass:

wherein, the piperazinyl polyether modified silicone oil is prepared by a method of 'preparation and compounding process of piperazinyl modified amino silicone oil' published by bin, Wandliang and Liuxupeng.

The composite emulsifier is a mixture of AEO-3 and AEO-9 which are commercially available in the conventional mass ratio.

The anti-agglomeration agent is conventional commercial peregal 0.

Glacial acetic acid is a conventional commercial product.

The deionized water is self-made.

Referring to fig. 1, the preparation process of silicone oil in the cylinder specifically comprises the following process steps:

step 1: mixing the piperazinyl polyether modified silicone oil and the composite emulsifier, and stirring for 30min to obtain an intermediate A;

step 2: adding a mixture of glacial acetic acid and 1/10 deionized water into the intermediate A, and stirring for 30min to obtain an intermediate B;

and step 3: dropwise adding the rest deionized water into the intermediate B at a constant speed for 120min to obtain an intermediate C;

and 4, step 4: and adding the anti-agglomeration agent into the intermediate C, and stirring for 10min to obtain the silicone oil in the cylinder.

Example 2

Example 2 differs from example 1 in that the piperazinyl polyether modified silicone oil prepared in preparation example 1 was used.

Example 3

Example 3 differs from example 2 in that the composite emulsifier is a mixture of a polyether silicone surfactant and oleyl alcohol polyoxyethylene ether mixed in a mass ratio of 3: 1.

And the structural general formula of the polyether organic silicon surfactant is as follows:

wherein n is an integer of 10-20, and the average molecular weight is 2120.

The oleyl alcohol polyoxyethylene ether is produced by Haian petrochemical industry in Jiangsu province, and has the HLB value of 8 and the hydroxyl value of 120-135.

Example 4

The difference between the embodiment 4 and the embodiment 3 is that the anti-agglomeration agent is fatty alcohol-polyoxyethylene ether silane, and the structural general formula of the fatty alcohol-polyoxyethylene ether silane is as follows:

wherein R2 is C12-C18 alkyl, and the average molecular weight is 3934.

Examples 5 to 10 differ from example 4 in that the mass percentages of the components in the silicone oil in the cylinder are as follows:

examples 11 to 15 differ from example 4 in that the source of the piperazinyl polyether modified silicone oil in each component of the silicone oil in the cylinder is as follows:

examples 16 to 20 differ from example 4 in that the mass percentages of the components of the silicone oil in the cylinder and the process parameters are as follows:

wherein the content of the first and second substances,

the alcohol ether carboxylic acid is obtained from Wuhan Huaqianjianke Biotechnology GmbH, and contains active substance 88 + -2%.

Cardanol polyoxyethylene ether was purchased from suzhou sailing biotechnology limited.

The isomeric alcohol polyoxyethylene ether is purchased from Haian of Jiangsu province, is prepared by chemical engineering and has the specification of E-1305.

The castor oil polyoxyethylene ether is purchased from Haian of Jiangsu province, is prepared by chemical engineering, and has a saponification value of 80-90 mgKOH/g.

Comparative example

The silicone oil used in comparative example 1 was a high concentration ultra stable softener 6628 from suzhou showpond chemical ltd.

Test method and test result

1. Stability against Heat

The experimental method comprises the following steps: preparing 50g/L of silicone oil working solution into a steel cup, adding 0.2g/L of disperse red 3B, preserving the temperature for 60 minutes at a certain temperature, pouring the working solution into a beaker after the temperature is maintained, and observing the stability.

The experimental results are reported in the following table:

an indication of no floc; as many as six indicate that there is a very small amount of floc; x represents a small amount of floc; and Xx indicates that much floc is present.

2. Electrolyte resistance (anhydrous sodium sulphate) stability

The experimental method comprises the following steps: preparing 50g/L of silicone oil working solution into a glass beaker, adding 0.2g/L of active B black, adding anhydrous sodium sulphate according to a certain concentration, preserving the temperature at 60 ℃ for 60 minutes, pouring out the working solution after the temperature is over, and observing the stability.

The experimental results are reported in the following table:

an indication of no floc; as many as six indicate that there is a very small amount of floc; x represents a small amount of floc; and Xx indicates that much floc is present.

3. Stability against acid/alkali

The experimental method comprises the following steps: preparing 50g/L of silicone oil working solution into a steel cup, adding 0.2g/L of disperse red 3BS, preserving the temperature at 130 ℃ for 90 minutes, pouring the working solution into a beaker after the temperature is over, and observing the stability.

The experimental results are reported in the following table:

an indication of no floc; as many as six indicate that there is a very small amount of floc; x represents a small amount of floc; and Xx indicates that much floc is present.

Conclusion

Compared with the common commercially available silicone oil, the silicone oil obtained by compounding the piperazinyl polyether modified silicone oil, the composite emulsifier, the glacial acetic acid, the anti-coagulant and the deionized water has better heat resistance, electrolyte resistance and acid and alkali resistance, is not easy to break emulsion, and better meets the requirements of cylinder entry.

On the other hand, compared with the addition of a general complex emulsifier and an anti-agglomeration agent, the addition of a complex emulsifier and an anti-agglomeration agent specifically selected in the present application limits the substance, molecular weight, and the like of the complex emulsifier and the anti-agglomeration agent, and can obtain more excellent effects and higher stability.

The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. Modifications and variations of this invention can be made without departing from its spirit and scope.