CN107523241B - Pre-coating type thread anti-loosening sealant and preparation method thereof - Google Patents

Abstract

The precoating type thread anti-loosening sealant comprises, by weight, 100 parts of a polymer-grade organic solvent, 75-102 parts of a comonomer, 0.075-0.2 part of an oil-soluble initiator and 45-140 parts of an environment-friendly organic solvent. The preparation method comprises the following steps: according to the proportion, uniformly stirring a polymer-grade organic solvent and a comonomer, adding an oil-soluble initiator, and stirring to obtain a mixture; after the oily initiator is dissolved, heating for heat preservation reaction; after the reaction is finished, a solid product is formed, unreacted comonomer and a polymerization-grade organic solvent in the solid product are separated, and the solid product is washed, filtered and dried in vacuum and then dissolved in an environment-friendly organic solvent to prepare the pre-coating type thread anti-loosening sealant. The thread sealant has the advantages of wide application range, low price, simple preparation method and process and strong practicability, can effectively seal all anti-leakage devices such as pipes and the like, is favorable for accelerating equipment assembly, reduces insurance cost and is convenient to maintain.

Description

A kind of pre-coated thread anti-loosening sealant and preparation method thereof

Technical field:

The invention belongs to the technical field of sealant preparation, in particular to a pre-coated thread anti-loosening sealant and a preparation method thereof.

Background technique:

Screws are indispensable industrial necessities in daily life: tiny screws for cameras, glasses, clocks, electronics, etc.; general screws for televisions, electrical products, musical instruments, furniture, etc.; large screws for engineering, construction, and bridges , nuts; transportation equipment, aircraft, trams, automobiles, etc. are used for large and small screws. The loosening of screws has always been a serious problem in industrial manufacturing and industrial products, and even a fatal hidden danger, and this irregular security accident has caused unpredictable changes in our daily life, work, transportation, national defense and military. harm. The anti-loosening technology of threaded fasteners has always been one of the research topics devoted to the engineering community. The early anti-loosening technology was mechanical methods such as the use of cotter pins, but due to the requirement of high machining accuracy, the use cost was high. Chemical locking and anti-loosening technology, which applies glue to the threads to prevent screw loosening, is an ideal choice.

The current commercially available thread anti-loosening sealants require a hot processing process when used, and improper operation may cause damage to the fasteners.

Invention content:

The purpose of the present invention is to overcome the deficiencies of the prior art, and to provide a pre-coated thread anti-loosening sealant and a preparation method thereof, which can be used after drying at room temperature to form a film without heating. It can not only prevent the fasteners from loosening due to external force, but also has a sealing effect, especially suitable for occasions with high sealing requirements. Because there is no need for on-site drip coating, the problems of missing coating, less coating, running and affecting the production cycle are avoided, so it is especially suitable for use in mass production assembly lines.

To achieve the above object, the present invention adopts the following technical solutions:

A pre-coated thread anti-loosening sealant, comprising the composition and the weight ratio of 100 parts of a polymer-grade organic solvent, 75 to 102 parts of a comonomer, 0.075 to 0.2 parts of an oil-soluble initiator, and 45 to 45 parts of an environment-friendly organic solvent. 140 servings.

The polymerization grade organic solvent is one of cyclohexane or chloroform.

The comonomer is a mixture of ethyl acrylate, styrene and maleic anhydride, and the weight ratio of the three is, ethyl acrylate: styrene: maleic anhydride=(60-80): (10-15): (5-7).

The oil-soluble initiator is benzoyl peroxide or azobisisobutyronitrile.

The environment-friendly organic solvent is a mixture of one or more of acetone, ethanol, butyl acetate or ethylene glycol ethyl ether acetate, and when it is a mixture of multiples, the proportioning is arbitrary.

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) according to the proportioning, in the reaction vessel, add polymerization grade organic solvent and comonomer successively, add oil-soluble initiator after stirring evenly, and continue stirring to form a mixture;

(2) After the oily initiator is dissolved, the mixture is heated to make the temperature rise to 70-80°C, and the reaction is kept for 6-8h;

(3) after the reaction is completed, form the solid product containing unreacted comonomer and polymerization grade organic solvent, after isolating unreacted comonomer and polymerization grade organic solvent in the solid product, the solid product is washed, filtered and vacuum drying;

(4) Dissolve the dried solid product in an environment-friendly organic solvent while stirring to prepare a product solution, which is a pre-coated thread anti-loosening sealant.

In the step (3), the vacuum drying conditions are: the vacuum degree is 0.05-0.1 MPa, the drying temperature is 90-100° C., and the drying time is 1-3 h.

For the pre-coated thread anti-loosening sealant prepared in the step (4), color paste is added to the pre-coated thread anti-loosening sealant according to color requirements to obtain a pre-coated thread anti-loosening sealant of the corresponding color, wherein : The color paste is oil-soluble color paste.

The mass fraction of the pre-coated thread anti-loosening sealant prepared in the step (4) is 40-60%.

The pre-coated thread anti-loosening sealant prepared in the step (4) can be repeatedly used more than 5 times at -40-80° C. after testing.

Beneficial effects of the present invention:

The technical scheme of the present invention is to prepare the polyacrylate copolymer by a heterogeneous solution polymerization method. The properties of the copolymer, such as hardness and elasticity, can be changed by adjusting the formula of the copolymer. The prepared thread sealant can not only play a role in sealing It can also effectively prevent the screws from loosening. The method of the invention is simple in production process, simple in use and operation, and strong in practicability.

Detailed ways:

The present invention will be further described in detail below in conjunction with the embodiments, and the principles and features of the present invention will be described below. The examples are only used to explain the present invention, and are not intended to limit the scope of the present invention.

Example 1

A pre-coated thread anti-loosening sealant, comprising the composition and weight ratio of 100 g of chloroform, 60 g of ethyl acrylate, 10 g of styrene, 5 g of maleic anhydride, 0.075 g of benzoyl peroxide and 45 g of acetone.

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) by proportioning, in reaction vessel, add chloroform 100g successively, ethyl acrylate 60g, styrene 10g and maleic anhydride 5g, add benzoyl peroxide 0.075g after stirring, and continue to stir to form mixture;

(2) After the benzoyl peroxide is dissolved, the mixture is heated to make the temperature rise to 70-75°C, and the reaction is incubated for 8h;

(3) after the completion of the reaction, the solid product containing unreacted chloroform, ethyl acrylate, styrene and maleic anhydride is formed, and the unreacted chloroform in the solid product is removed under reduced pressure, ethyl acrylate, styrene and After maleic anhydride, the solid product was washed with water, filtered and dried under vacuum. The vacuum drying conditions were: vacuum degree was 0.05MPa, drying temperature was 90°C, and drying time was 3h;

(4) Dissolve the dried solid product in acetone while stirring, and prepare a product solution, which is a pre-coating thread anti-loosening sealant, and the mass fraction of the pre-coating thread anti-loosening sealant is 60%, According to the color requirements, add 1% blue paste of sealant to the pre-coated thread anti-loosening sealant to obtain blue pre-coated thread anti-loosening sealant. Test, it can be reused more than 5 times at -40 ~ 80 ℃.

Example 2

A pre-coated thread anti-loosening sealant, comprising the composition and weight ratio of 100 g of chloroform, 70 g of ethyl acrylate, 10 g of styrene, 6 g of maleic anhydride, 0.1 g of benzoyl peroxide and 80 g of ethanol.

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) by proportioning, in reaction vessel, add chloroform 100g successively, ethyl acrylate 70g, styrene 10g and maleic anhydride 6g, after stirring, add benzoyl peroxide 0.1g, and continue to stir to form mixture;

(2) After the benzoyl peroxide is dissolved, the mixture is heated to make the temperature rise to 70-75°C, and the reaction is incubated for 7h;

(3) after the completion of the reaction, the solid product containing unreacted chloroform, ethyl acrylate, styrene and maleic anhydride is formed, and the unreacted chloroform in the solid product is removed under reduced pressure, ethyl acrylate, styrene and After maleic anhydride, the solid product was washed with water, filtered and dried in vacuum. The vacuum drying conditions were: vacuum degree was 0.06MPa, drying temperature was 100°C, and drying time was 2h;

(4) Dissolve the dried solid product in ethanol while stirring, and prepare a product solution, which is a pre-coating thread anti-loosening sealant, and the mass fraction of the pre-coating thread anti-loosening sealant is 50%, According to the color requirements, add 1% yellow paste of sealant to the pre-coated thread anti-loosening sealant to obtain a yellow pre-coated thread anti-loosening sealant, and test the prepared pre-coated thread anti-loosening sealant. It can be reused more than 5 times at -40～80℃.

Example 3

A pre-coated thread anti-loosening sealant, comprising the composition and weight ratio of 100 g of chloroform, 80 g of ethyl acrylate, 15 g of styrene and 7 g of maleic anhydride, 0.2 g of azobisisobutyronitrile and 140 g of ethanol .

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) by proportioning, in the reaction vessel, successively add chloroform 100g, ethyl acrylate 80g, styrene 15g and maleic anhydride 7g, after stirring, add azobisisobutyronitrile 0.2g, and continue to stir to form a mixture ;

(2) After the azobisisobutyronitrile is dissolved, the mixture is heated to make the temperature rise to 75-80°C, and the reaction is kept for 7h;

(3) after the completion of the reaction, the solid product containing unreacted chloroform, ethyl acrylate, styrene and maleic anhydride is formed, and the unreacted chloroform in the solid product is removed under reduced pressure, ethyl acrylate, styrene and After maleic anhydride, the solid product was washed with water, filtered and dried in vacuum. The vacuum drying conditions were: vacuum degree was 0.1MPa, drying temperature was 100°C, and drying time was 1h;

(4) Dissolve the dried solid product in ethanol while stirring to prepare a product solution, which is a pre-coated thread anti-loosening sealant, and the mass fraction of the pre-coated thread anti-loosening sealant is 40%, According to the color requirements, add 1% red paste of sealant to the pre-coated thread anti-loosening sealant to obtain a red pre-coated thread anti-loosening sealant, and test the prepared pre-coated thread anti-loosening sealant. It can be reused more than 5 times at -40～80℃.

Example 4

A pre-coated thread anti-loosening sealant, comprising the composition and weight ratio of 100 g of cyclohexane, 80 g of ethyl acrylate, 10 g of styrene and 5 g of maleic anhydride, 0.1 g of azobisisobutyronitrile and butyl acetate 130g of mixed solvent with the ratio of ester and ethylene glycol ether acetate being 1:1.

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) according to proportioning, add cyclohexane 100g, ethyl acrylate 80g, styrene 10g and maleic anhydride 5g successively in reaction vessel, add azobisisobutyronitrile 0.1g after stirring, and continue to stir to form mixture ;

(2) After the azobisisobutyronitrile is dissolved, the mixture is heated to make the temperature rise to 75-80°C, and the reaction is kept for 7h;

(3) after the completion of the reaction, the solid product containing unreacted cyclohexane, ethyl acrylate, styrene and maleic anhydride is formed, and the unreacted cyclohexane in the solid product is removed under reduced pressure, ethyl acrylate, styrene and After maleic anhydride, the solid product was washed with water, filtered and dried under vacuum. The vacuum drying conditions were: vacuum degree was 0.08MPa, drying temperature was 100°C, and drying time was 1.5h;

(4) Dissolve the dried solid product in a mixed solvent of butyl acetate and ethylene glycol ether acetate while stirring, and prepare a product solution, which is a pre-coating thread anti-loosening sealant. The mass fraction of the pre-coated thread anti-loosening sealant is 40%. According to the color requirements, add 1% white paste of the sealant to the pre-coated thread anti-loosening sealant to obtain a white pre-coated thread anti-loosening sealant. The pre-coated thread anti-loosening sealant was tested, and it can be reused more than 5 times at -40 ~ 80 ℃.

Example 5

A pre-coated thread anti-loosening sealant, comprising the composition and weight ratio of 100 g of cyclohexane, 80 g of ethyl acrylate, 10 g of styrene and 5 g of maleic anhydride, 0.1 g of azobisisobutyronitrile and 70 g of acetone .

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) according to proportioning, add cyclohexane 100g, ethyl acrylate 80g, styrene 10g and maleic anhydride 5g successively in reaction vessel, add azobisisobutyronitrile 0.1g after stirring, and continue to stir to form mixture ;

(2) After the azobisisobutyronitrile is dissolved, the mixture is heated to make the temperature rise to 75-80°C, and the reaction is incubated for 6h;

(3) after the completion of the reaction, the solid product containing unreacted cyclohexane, ethyl acrylate, styrene and maleic anhydride is formed, and the unreacted cyclohexane in the solid product is removed under reduced pressure, ethyl acrylate, styrene and After maleic anhydride, the solid product was washed with water, filtered and dried under vacuum. The vacuum drying conditions were: vacuum degree was 0.08MPa, drying temperature was 90°C, and drying time was 2.5h;

(4) Dissolve the dried solid product in acetone while stirring, and prepare a product solution, which is a pre-coating thread anti-loosening sealant, and the mass fraction of the pre-coating thread anti-loosening sealant is 55%, According to the color requirements, add 1% white paste of sealant to the pre-coated thread anti-loosening sealant to obtain a white pre-coated thread anti-loosening sealant, and test the prepared pre-coated thread anti-loosening sealant. It can be reused more than 5 times at -40～80℃.

Example 6

A pre-coated thread anti-loosening sealant, comprising the composition and weight ratio of 100 g of cyclohexane, 60 g of ethyl acrylate, 15 g of styrene and 7 g of maleic anhydride, 0.15 g of azobisisobutyronitrile and 75 g of acetone .

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) by proportioning, in the reaction vessel, successively add cyclohexane 100g, ethyl acrylate 60g, styrene 15g and maleic anhydride 7g, add azobisisobutyronitrile 0.15g after stirring, and continue stirring to form a mixture ;

(2) After azobisisobutyronitrile, the mixture is heated to make the temperature rise to 75-80°C, and the reaction is kept for 6h;

(3) after the completion of the reaction, the solid product containing unreacted cyclohexane, ethyl acrylate, styrene and maleic anhydride is formed, and the unreacted cyclohexane in the solid product is removed under reduced pressure, ethyl acrylate, styrene and After maleic anhydride, the solid product was washed with water, filtered and dried under vacuum. The vacuum drying conditions were: vacuum degree was 0.06MPa, drying temperature was 95°C, and drying time was 3h;

(4) Dissolve the dried solid product in acetone while stirring to prepare a product solution, which is a pre-coated thread anti-loosening sealant, and the mass fraction of the pre-coated thread anti-loosening sealant is 50%, According to the color requirements, add 1% white paste of sealant to the pre-coated thread anti-loosening sealant to obtain a white pre-coated thread anti-loosening sealant, and test the prepared pre-coated thread anti-loosening sealant. It can be reused more than 5 times at -40～80℃.

Example 7

A pre-coated thread anti-loosening sealant, comprising the composition and weight ratio of 100 g of cyclohexane, 80 g of ethyl acrylate, 10 g of styrene, 7 g of maleic anhydride, 0.2 g of benzoyl peroxide and 110 g of ethanol.

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) by proportioning, in reaction vessel, successively add cyclohexane 100g, ethyl acrylate 80g, styrene 10g and maleic anhydride 7g, add benzoyl peroxide 0.2g after stirring, and continue to stir to form mixture;

(2) After the benzoyl peroxide is dissolved, the mixture is heated to make the temperature rise to 70-75°C, and the reaction is incubated for 7h;

(3) after the completion of the reaction, the solid product containing unreacted cyclohexane, ethyl acrylate, styrene and maleic anhydride is formed, and the unreacted cyclohexane in the solid product is removed under reduced pressure, ethyl acrylate, styrene and After maleic anhydride, the solid product was washed with water, filtered and dried under vacuum. The vacuum drying conditions were: vacuum degree was 0.05MPa, drying temperature was 95°C, and drying time was 1h;

(4) Dissolve the dried solid product in ethanol while stirring, and prepare a product solution, which is a pre-coating thread anti-loosening sealant, and the mass fraction of the pre-coating thread anti-loosening sealant is 44%, According to the color requirements, add 1% white paste of sealant to the pre-coated thread anti-loosening sealant to obtain a white pre-coated thread anti-loosening sealant, and test the prepared pre-coated thread anti-loosening sealant. It can be reused more than 5 times at -40～80℃.

Example 8

A pre-coated thread anti-loosening sealant, comprising the composition and weight ratio of 100 g of chloroform, 80 g of ethyl acrylate, 10 g of styrene, 7 g of maleic anhydride, 0.2 g of benzoyl peroxide and 110 g of ethanol.

The preparation method of the pre-coated thread anti-loosening sealant comprises the following steps:

(1) by proportioning, in reaction vessel, add chloroform 100g successively, ethyl acrylate 80g, styrene 10g and maleic anhydride 7g, add benzoyl peroxide 0.2g after stirring, and continue to stir to form mixture;

(2) After the benzoyl peroxide is dissolved, the mixture is heated to make the temperature rise to 70-75°C, and the reaction is incubated for 7h;

(3) after the completion of the reaction, the solid product containing unreacted chloroform, ethyl acrylate, styrene and maleic anhydride is formed, and the unreacted chloroform in the solid product is removed under reduced pressure, ethyl acrylate, styrene and After maleic anhydride, the solid product was washed with water, filtered and dried under vacuum. The vacuum drying conditions were: vacuum degree was 0.1MPa, drying temperature was 100°C, and drying time was 2h;

(4) Dissolve the dried solid product in ethanol while stirring, and prepare a product solution, which is a pre-coating thread anti-loosening sealant, and the mass fraction of the pre-coating thread anti-loosening sealant is 44%, According to the color requirements, add 1% white paste of sealant to the pre-coated thread anti-loosening sealant to obtain a white pre-coated thread anti-loosening sealant, and test the prepared pre-coated thread anti-loosening sealant. It can be reused more than 5 times at -40～80℃.

The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection of the present invention. within the range.

Claims (1)

1. a preparation method of pre-coating type thread anti-loosening sealant, it is characterized in that, described pre-coating type thread anti-loosening sealant comprises composition and its weight ratio are, 100 parts of polymeric grade organic solvents, comonomers. 75～102 parts, 0.075～0.2 parts of oil-soluble initiator and 45～140 parts of environment-friendly organic solvent, described polymerization grade organic solvent is a kind of in cyclohexane or chloroform, described comonomer is The mixture of ethyl acrylate, styrene and maleic anhydride, the weight ratio of the three is, ethyl acrylate: styrene: maleic anhydride = (60-80): (10-15): (5-7), so Described oil-soluble initiator is benzoyl peroxide or azobisisobutyronitrile, and its addition amount is 0.1～0.2% of the total amount of comonomer, and described environment-friendly organic solvent is acetone, ethanol, butyl acetate Or one or more mixtures in ethylene glycol ethyl ether acetate, when it is multiple mixtures, the proportioning is any ratio; The preparation method specifically includes the following steps: (1) according to the proportioning, in the reaction vessel, add polymerization grade organic solvent and comonomer successively, add oil-soluble initiator after stirring evenly, and continue stirring to form a mixture; (2) After the oily initiator is dissolved, the mixture is heated to make the temperature rise to 70-80°C, and the reaction is kept for 6-8h; (3) after the completion of the reaction, the solid product containing unreacted comonomer and polymerization-grade organic solvent is formed, after the unreacted comonomer and polymerization-grade organic solvent in the solid product are removed under reduced pressure, the solid product is washed with water, filtered and vacuum drying, the vacuum degree is 0.05～0.1MPa, the drying temperature is 90～100℃, and the drying time is 1～3h; (4) Dissolve the dried solid product in an environmentally friendly organic solvent while stirring, and prepare a product solution, which is a pre-coating thread anti-loosening sealant. The mass fraction of the pre-coating thread anti-loosening sealant is: 40~60%, according to the color requirements, add color paste to the pre-coated thread anti-loosening sealant to obtain the pre-coated thread anti-loosening sealant of the corresponding color, wherein: the color paste is oil-soluble color paste, According to the test, the pre-coated thread anti-loosening sealant can be reused more than 5 times at -40~80℃.