CN105294748A - Acrylate self-lubricating monomer with molecular chain containing boron and application and preparation method thereof - Google Patents

Acrylate self-lubricating monomer with molecular chain containing boron and application and preparation method thereof Download PDF

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CN105294748A
CN105294748A CN201510791450.1A CN201510791450A CN105294748A CN 105294748 A CN105294748 A CN 105294748A CN 201510791450 A CN201510791450 A CN 201510791450A CN 105294748 A CN105294748 A CN 105294748A
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self
type monomer
water
lubricating type
boric acid
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艾少华
赵景左
韩胜利
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HUBEI HUITIAN ADHESIVE ENTERPRISE CO Ltd
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HUBEI HUITIAN ADHESIVE ENTERPRISE CO Ltd
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Abstract

The invention discloses an acrylate self-lubricating monomer with a molecular chain containing boron and an application and a preparation method thereof. The invention relates to the field of acrylate monomer. The structural formula of the self-lubricating monomer is as shown in the (I), wherein the structure of at least one of R1, R2 and R3 is (II); R4 is alkyl group or substituted alkyl group having at least one carbon chain; and R5 is hydrogen, an alkyl group or a substituted alkyl group. By introducing boron into the main chain of the acrylate monomer, the acrylate monomer is endowed with self-lubricating performance. During the preparation process of anaerobic adhesive, the self-lubricating monomer used as a main reaction monomer undergoes a free radical polymerization reaction so as to form a thermoplastic elastomer polymer with a long and amorphous linear molecular chain.

Description

The acrylate self-lubricating type monomer of boracic and purposes, preparation method on molecular chain
Technical field
The present invention relates to acrylate monomer field, acrylate self-lubricating type monomer specifically relating to boracic on a kind of molecular chain and uses thereof, preparation method.
Background technology
Acrylic ester polymer used for anaerobic adhesive is for principal monomer with the alkyl ester of acrylic or methacrylic acid, the polyreaction of free radical is carried out, the thermoplastic elastomer polymer of the long and unbodied linear molecule chain of formation by two or more reaction monomers.At present, monomer normally monoacrylate monomers, monoacrylate monomers, diacrylate monomer, diacrylate monomer, the triacrylate monomer etc. that acrylic ester polymer used for anaerobic adhesive uses are prepared.
The monomer that existing acrylic ester polymer used for anaerobic adhesive uses also exists the shortcoming of poor lubricity, therefore existing anaerobic glue poor lubricity, and after gluing, fastening piece frictional coefficient increases, and torque coefficient can significantly rise.Torque coefficient K is the significant data that bolt tightens in process, and it determines primarily of the frictional coefficient of fastening piece.Known according to T=KDF (T is tightening torque, and D is nominal diameter, and F is clamping force), for obtaining the clamping force of regulation, need significantly to promote tightening torque, this brings larger trouble can to the assembly technology of a lot of client.
Summary of the invention
The object of the invention is the deficiency in order to overcome above-mentioned background technology, acrylate self-lubricating type monomer providing boracic on a kind of molecular chain and preparation method thereof, boron is introduced acrylate monomer main chain by the present invention, makes acrylate monomer possess self-lubricating property.
The invention provides the acrylate self-lubricating type monomer of boracic on a kind of molecular chain, the structural formula of this self-lubricating type monomer, as shown in (I), wherein has the structure of at least for (II) in R1, R2, R3,
R4 is the alkyl or the substituted alkyl that have a carbochain at least, and R5 is hydrogen, alkyl or substituted alkyl.
On the basis of technique scheme, the structural formula of described self-lubricating type monomer is:
or
Described self-lubricating type monomer is mixed by the isomers of following 4 kinds of structures:
On the basis of technique scheme, the structural formula of described self-lubricating type monomer is:
or
or
Described self-lubricating type monomer is mixed by the isomers of following 3 kinds of structures:
The present invention also provides the purposes of the acrylate self-lubricating type monomer of boracic on above-mentioned molecular chain, in the preparation process of anaerobic glue, this self-lubricating type monomer is as main reaction monomers, by the polyreaction of free radical, form the thermoplastic elastomer polymer of long and unbodied linear molecule chain.
The present invention also provides the preparation method of the acrylate self-lubricating type monomer of boracic on above-mentioned molecular chain, comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system; Prepare basic raw material: boric acid, hydroxy acrylate, wherein, the mol ratio of boric acid and hydroxy acrylate is 1:3; Drop into boric acid and hydroxy acrylate, add the stopper of total amount 0.05% ~ 0.5%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C ~ 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collects cut water and weighs, when the quality of cut water reaches theoretical reaction water growing amount, stop heating and pressure release, cooling, obtains the acrylate self-lubricating type monomer of boracic on molecular chain.
On the basis of technique scheme, the structural formula of described self-lubricating type monomer is
time,
The preparation process of this self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, prepares basic raw material: boric acid, hydroxyethyl methylacrylate; 1:3 drops into boric acid and hydroxyethyl methylacrylate in molar ratio, add the stopper of total amount 0.05%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collects cut water and weighs, when the quality of cut water reaches theoretical reaction water growing amount, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer;
When described self-lubricating type monomer is mixed by the isomers of following 4 kinds of structures:
The preparation process of described self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, and prepare basic raw material: boric acid, Rocryl 410, wherein, the mol ratio of boric acid and Rocryl 410 is 1:3; Drop into boric acid and Rocryl 410, add the stopper of total amount 0.5%Wt again, stirring heats up and be incubated carries out esterification at 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collects cut water and weighs, when the quality of cut water reaches theoretical reaction water growing amount, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer.
On the basis of technique scheme, described stopper is any one in Resorcinol, 1,4-naphthoquinone, 2,4 dimethyl 6 tert butyl phenol, MEHQ.
The present invention also provides the preparation method of the acrylate self-lubricating type monomer of boracic on above-mentioned molecular chain, comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, alcohol, hydroxy acrylate, the concrete structure formula according to self-lubricating type monomer to be prepared determines charging capacity: boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, drop into boric acid and hydroxy acrylate, add the stopper of total amount 0.05% ~ 0.5%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C ~ 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into alcohol again, continue to vacuumize, reaction conditions is constant, continue collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtain the acrylate self-lubricating type monomer of boracic on molecular chain.
On the basis of technique scheme, the structural formula of described self-lubricating type monomer is
time;
The preparation process of this self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, ethylene glycol, hydroxyethyl methylacrylate, concrete structure formula according to self-lubricating type monomer to be prepared determines charging capacity: boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, determines that the mol ratio of boric acid, ethylene glycol, hydroxyethyl methylacrylate is 1:1:2; Drop into boric acid and hydroxyethyl methylacrylate, add the stopper of total amount 0.05%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water also to weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into ethylene glycol, continue to vacuumize, reaction conditions is constant, continues collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer;
The structural formula of described self-lubricating type monomer is
time;
The preparation process of this self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, ethylene glycol, hydroxyethyl methylacrylate, wherein, boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, and the mol ratio of boric acid, ethylene glycol, hydroxyethyl methylacrylate is 1:1:1; Drop into boric acid and hydroxyethyl methylacrylate, add the stopper of total amount 0.25%Wt again, stirring heats up and be incubated carries out esterification at 110 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water also to weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into Diethylene Glycol, continue to vacuumize, reaction conditions is constant, collects cut water and weighs, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer;
When described self-lubricating type monomer is mixed by the isomers of following 3 kinds of structures:
The preparation process of this self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, Diethylene Glycol, Rocryl 410, concrete structure formula according to self-lubricating type monomer to be prepared determines charging capacity: boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, determines that the mol ratio of boric acid, Diethylene Glycol, Rocryl 410 is 1:1:2; Drop into boric acid and Rocryl 410, add the stopper of total amount 0.5%Wt again, stirring heats up and be incubated carries out esterification at 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water also to weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into Diethylene Glycol, continue to vacuumize, reaction conditions is constant, collects cut water and weighs, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer.
On the basis of technique scheme, described stopper is any one in Resorcinol, 1,4-naphthoquinone, 2,4 dimethyl 6 tert butyl phenol, MEHQ.
Compared with prior art, advantage of the present invention is as follows:
Boron-containing compound has excellent lubricity, and boron is introduced acrylate monomer main chain by the present invention, makes acrylate monomer possess self-lubricating property.On molecular chain prepared by the present invention, the acrylate self-lubricating type monomer of boracic can add in anaerobic glue, makes anaerobic glue possess lubricity, reduces its frictional coefficient, be conducive to assembly technology.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
The content of each composition in the embodiment of the present invention, if not otherwise specified, all in mass percent Wt.
The embodiment of the present invention provides the acrylate self-lubricating type monomer of boracic on a kind of molecular chain, the structural formula of this self-lubricating type monomer is as shown in (I), wherein has the structure of in R1, R2, R3 at least for (II), R4 is the alkyl or the substituted alkyl that have a carbochain at least, R5 is hydrogen, alkyl or substituted alkyl, this self-lubricating type monomer is obtained by esterification by boric acid and hydroxy acrylate, or is obtained by esterification by boric acid, alcohol, hydroxy acrylate.
The embodiment of the present invention provides the purposes of the acrylate self-lubricating type monomer of boracic on above-mentioned molecular chain: this self-lubricating type monomer can based on polymkeric substance, for the preparation of anaerobic glue.In the preparation process of anaerobic glue, this self-lubricating type monomer, as main reaction monomers, by the polyreaction of free radical, forms the thermoplastic elastomer polymer of long and unbodied linear molecule chain.
The embodiment of the present invention also provides the preparation method of the acrylate self-lubricating type monomer of boracic on above-mentioned molecular chain, comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system; According to the different structure formula of self-lubricating type monomer to be prepared, can adopt and prepare this self-lubricating type monomer in two ways:
Mode one: prepare basic raw material: boric acid, hydroxy acrylate, wherein, the mol ratio of boric acid and hydroxy acrylate is 1:3; Drop into boric acid and hydroxy acrylate, add the stopper of total amount 0.05% ~ 0.5%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C ~ 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collects cut water and weighs, when the quality of cut water reaches theoretical reaction water growing amount, stop heating and pressure release, cooling, obtains the self-lubricating type monomer of counter structure formula;
Mode two: prepare basic raw material: boric acid, alcohol, hydroxy acrylate, the concrete structure formula according to self-lubricating type monomer to be prepared determines charging capacity: boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, drop into boric acid and hydroxy acrylate, add the stopper of total amount 0.05% ~ 0.5%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C ~ 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into alcohol again, continue to vacuumize, reaction conditions is constant, continue collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtain the self-lubricating type monomer of counter structure formula.
Stopper can be any one in Resorcinol, 1,4-naphthoquinone, 2,4 dimethyl 6 tert butyl phenol, MEHQ.
Below by 6 specific embodiments, acrylate self-lubricating type monomer of boracic on the molecular chain in the present invention and preparation method thereof is described in detail.
Embodiment 1:
The acrylate self-lubricating type monomer of boracic on the molecular chain that the present embodiment provides, its structural formula is:
The preparation method of this self-lubricating type monomer comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system, and prepare basic raw material: boric acid, hydroxyethyl methylacrylate, wherein, the mol ratio of boric acid and hydroxy acrylate is 1:3; 1:3 drops into boric acid and hydroxyethyl methylacrylate in molar ratio, add the Resorcinol (stopper) of total amount 0.05%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collects cut water and weighs, when the quality of cut water reaches theoretical reaction water growing amount, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer.
Embodiment 2:
The self-lubricating type monomer structure formula that the present embodiment provides is identical with the self-lubricating type monomer structure formula in embodiment 1, and the preparation method of this self-lubricating type monomer comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system, and prepare basic raw material: boric acid, hydroxyethyl methylacrylate, wherein, the mol ratio of boric acid and hydroxy acrylate is 1:3; 1:3 drops into boric acid and hydroxyethyl methylacrylate in molar ratio, add 1 of total amount 0.25%Wt again, 4-naphthoquinones (stopper), stirring heats up and be incubated carries out esterification at 110 DEG C, vacuumizes and dewaters, water vapour is back to water separator after condenser, collect cut water and weigh, when the quality of cut water reaches theoretical reaction water growing amount, stopping heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer.
Embodiment 3:
The acrylate self-lubricating type monomer of boracic on the molecular chain that the present embodiment provides, its structural formula is:
The preparation method of this self-lubricating type monomer comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, ethylene glycol, hydroxyethyl methylacrylate, wherein, boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, and the mol ratio of boric acid, ethylene glycol, hydroxyethyl methylacrylate is 1:1:2, drop into boric acid and hydroxyethyl methylacrylate, add the MEHQ (stopper) of total amount 0.05%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into ethylene glycol, continue to vacuumize, reaction conditions is constant, continue collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtain above-mentioned self-lubricating type monomer.
Embodiment 4:
The acrylate self-lubricating type monomer of boracic on the molecular chain that the present embodiment provides, its structural formula is:
The preparation method of this self-lubricating type monomer comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, Diethylene Glycol, Rocryl 410, its mesoboric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, and the mol ratio of boric acid, Diethylene Glycol, Rocryl 410 is 1:1:2, drop into boric acid and Rocryl 410, add 1 of total amount 0.5%Wt again, 4-naphthoquinones (stopper), stirring heats up and be incubated carries out esterification at 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into Diethylene Glycol, continue to vacuumize, reaction conditions is constant, collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtain above-mentioned self-lubricating type monomer.
Embodiment 5:
The acrylate self-lubricating type monomer of boracic on the molecular chain that the present embodiment provides, its structural formula is:
The preparation method of this self-lubricating type monomer comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system, and prepare basic raw material: boric acid, Rocryl 410, wherein, the mol ratio of boric acid and hydroxy acrylate is 1:3; 1:3 drops into boric acid and Rocryl 410 in molar ratio, add 2 of total amount 0.5%Wt again, 4-dimethyl-6-tert.-butyl phenol (stopper), stirring heats up and be incubated carries out esterification at 130 DEG C, vacuumizes and dewaters, water vapour is back to water separator after condenser, collect cut water and weigh, when the quality of cut water reaches theoretical reaction water growing amount, stopping heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer.
Embodiment 6:
The acrylate self-lubricating type monomer of boracic on the molecular chain that the present embodiment provides, its structural formula is:
The preparation method of this self-lubricating type monomer comprises the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, ethylene glycol, hydroxyethyl methylacrylate, wherein, boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, and the mol ratio of boric acid, ethylene glycol, hydroxyethyl methylacrylate is 1:1:1, drop into boric acid and hydroxyethyl methylacrylate, add the Resorcinol (stopper) of total amount 0.25%Wt again, stirring heats up and be incubated carries out esterification at 110 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into Diethylene Glycol, continue to vacuumize, reaction conditions is constant, collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtain above-mentioned self-lubricating type monomer.
Those skilled in the art can carry out various modifications and variations to the embodiment of the present invention, if these amendments and modification are within the scope of the claims in the present invention and equivalent technologies thereof, then these revise and modification also within protection scope of the present invention.
The prior art that the content do not described in detail in specification sheets is known to the skilled person.

Claims (10)

1. the acrylate self-lubricating type monomer of boracic on molecular chain, is characterized in that: the structural formula of this self-lubricating type monomer, as shown in (I), wherein has the structure of at least for (II) in R1, R2, R3,
R4 is the alkyl or the substituted alkyl that have a carbochain at least, and R5 is hydrogen, alkyl or substituted alkyl.
2. the acrylate self-lubricating type monomer of boracic on molecular chain as claimed in claim 1, it is characterized in that, the structural formula of described self-lubricating type monomer is:
or
Described self-lubricating type monomer is mixed by the isomers of following 4 kinds of structures:
3. the acrylate self-lubricating type monomer of boracic on molecular chain as claimed in claim 1, it is characterized in that, the structural formula of described self-lubricating type monomer is:
or
Described self-lubricating type monomer is mixed by the isomers of following 3 kinds of structures:
4. the as claimed any one in claims 1 to 3 purposes of the acrylate self-lubricating type monomer of boracic on molecular chain, it is characterized in that: in the preparation process of anaerobic glue, this self-lubricating type monomer is as main reaction monomers, by the polyreaction of free radical, form the thermoplastic elastomer polymer of long and unbodied linear molecule chain.
5. the as claimed any one in claims 1 to 3 preparation method of the acrylate self-lubricating type monomer of boracic on molecular chain, is characterized in that, comprise the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system; Prepare basic raw material: boric acid, hydroxy acrylate, wherein, the mol ratio of boric acid and hydroxy acrylate is 1:3; Drop into boric acid and hydroxy acrylate, add the stopper of total amount 0.05% ~ 0.5%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C ~ 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collects cut water and weighs, when the quality of cut water reaches theoretical reaction water growing amount, stop heating and pressure release, cooling, obtains the acrylate self-lubricating type monomer of boracic on molecular chain.
6. the preparation method of the acrylate self-lubricating type monomer of boracic on molecular chain as claimed in claim 5, it is characterized in that, the structural formula of described self-lubricating type monomer is
time,
The preparation process of this self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, prepares basic raw material: boric acid, hydroxyethyl methylacrylate; 1:3 drops into boric acid and hydroxyethyl methylacrylate in molar ratio, add the stopper of total amount 0.05%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collects cut water and weighs, when the quality of cut water reaches theoretical reaction water growing amount, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer;
When described self-lubricating type monomer is mixed by the isomers of following 4 kinds of structures:
The preparation process of described self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, and prepare basic raw material: boric acid, Rocryl 410, wherein, the mol ratio of boric acid and Rocryl 410 is 1:3; Drop into boric acid and Rocryl 410, add the stopper of total amount 0.5%Wt again, stirring heats up and be incubated carries out esterification at 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collects cut water and weighs, when the quality of cut water reaches theoretical reaction water growing amount, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer.
7. the preparation method of the acrylate self-lubricating type monomer of boracic on the molecular chain according to any one of claim 5 or 6, it is characterized in that: described stopper is Resorcinol, 1, any one in 4-naphthoquinones, 2,4 dimethyl 6 tert butyl phenol, MEHQ.
8. the as claimed any one in claims 1 to 3 preparation method of the acrylate self-lubricating type monomer of boracic on molecular chain, is characterized in that, comprise the following steps:
Reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, alcohol, hydroxy acrylate, the concrete structure formula according to self-lubricating type monomer to be prepared determines charging capacity: boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, drop into boric acid and hydroxy acrylate, add the stopper of total amount 0.05% ~ 0.5%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C ~ 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into alcohol again, continue to vacuumize, reaction conditions is constant, continue collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtain the acrylate self-lubricating type monomer of boracic on molecular chain.
9. the preparation method of the acrylate self-lubricating type monomer of boracic on molecular chain as claimed in claim 8, it is characterized in that, the structural formula of described self-lubricating type monomer is
time;
The preparation process of this self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, ethylene glycol, hydroxyethyl methylacrylate, concrete structure formula according to self-lubricating type monomer to be prepared determines charging capacity: boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, determines that the mol ratio of boric acid, ethylene glycol, hydroxyethyl methylacrylate is 1:1:2; Drop into boric acid and hydroxyethyl methylacrylate, add the stopper of total amount 0.05%Wt again, stirring heats up and be incubated carries out esterification at 80 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water also to weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into ethylene glycol, continue to vacuumize, reaction conditions is constant, continues collect cut water and weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer;
The structural formula of described self-lubricating type monomer is
time;
The preparation process of this self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, ethylene glycol, hydroxyethyl methylacrylate, wherein, boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, and the mol ratio of boric acid, ethylene glycol, hydroxyethyl methylacrylate is 1:1:1; Drop into boric acid and hydroxyethyl methylacrylate, add the stopper of total amount 0.25%Wt again, stirring heats up and be incubated carries out esterification at 110 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water also to weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into Diethylene Glycol, continue to vacuumize, reaction conditions is constant, collects cut water and weighs, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer;
When described self-lubricating type monomer is mixed by the isomers of following 3 kinds of structures:
The preparation process of this self-lubricating type monomer is as follows: reaction vessel is in series with water separator, condenser, vacuum system, prepare basic raw material: boric acid, Diethylene Glycol, Rocryl 410, concrete structure formula according to self-lubricating type monomer to be prepared determines charging capacity: boric acid is 1:3 with the mol ratio participating in the total hydroxyl reacted in theory, determines that the mol ratio of boric acid, Diethylene Glycol, Rocryl 410 is 1:1:2; Drop into boric acid and Rocryl 410, add the stopper of total amount 0.5%Wt again, stirring heats up and be incubated carries out esterification at 130 DEG C, vacuumize and dewater, water vapour is back to water separator after condenser, collect cut water also to weigh, when the weight of cut water reach this walk theoretical reaction water growing amount time, pressure release, drop into Diethylene Glycol, continue to vacuumize, reaction conditions is constant, collects cut water and weighs, when the weight of cut water reach this walk theoretical reaction water growing amount time, stop heating and pressure release, cooling, obtains above-mentioned self-lubricating type monomer.
10. the as claimed in claim 8 or 9 preparation method of the acrylate self-lubricating type monomer of boracic on molecular chain, it is characterized in that: described stopper is Resorcinol, 1, any one in 4-naphthoquinones, 2,4 dimethyl 6 tert butyl phenol, MEHQ.
CN201510791450.1A 2015-11-17 2015-11-17 Acrylate self-lubricating monomer with molecular chain containing boron and application and preparation method thereof Pending CN105294748A (en)

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CN106752985A (en) * 2016-12-14 2017-05-31 湖北回天新材料股份有限公司 A kind of quick detachable controllable thread friction coefficient anaerobic adhesive and preparation method thereof
CN109054737A (en) * 2018-07-25 2018-12-21 佛山皖阳生物科技有限公司 A kind of preparation method of the moisture-proof starch anaerobic adhesive of stable type
CN113024700A (en) * 2021-03-08 2021-06-25 常州时创能源股份有限公司 Sprayable boron source for silicon wafer boron diffusion and application thereof

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CN106752985A (en) * 2016-12-14 2017-05-31 湖北回天新材料股份有限公司 A kind of quick detachable controllable thread friction coefficient anaerobic adhesive and preparation method thereof
CN109054737A (en) * 2018-07-25 2018-12-21 佛山皖阳生物科技有限公司 A kind of preparation method of the moisture-proof starch anaerobic adhesive of stable type
CN113024700A (en) * 2021-03-08 2021-06-25 常州时创能源股份有限公司 Sprayable boron source for silicon wafer boron diffusion and application thereof

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Application publication date: 20160203