CN105175598A - Synthesis method of SMA resin with low molecular weight - Google Patents
Synthesis method of SMA resin with low molecular weight Download PDFInfo
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- CN105175598A CN105175598A CN201510493713.0A CN201510493713A CN105175598A CN 105175598 A CN105175598 A CN 105175598A CN 201510493713 A CN201510493713 A CN 201510493713A CN 105175598 A CN105175598 A CN 105175598A
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Abstract
The present invention provides a synthesis method of an SMA resin with low molecular weight. The method comprises the steps of: 1, selecting starting materials a, b and c in a certain amount, adding the starting materials to a dropping tank A, a dropping tank B and a dropping tank C; 2, heating the reaction kettle to reflux, dropwise adding the components in the dropping tank A, dropping tank B and dropping tank C uniformly into a reactor, and stirring at constant speed for 2-4 h; and 3, after the addition, maintaining the reflux state for 1-2 h, then introducing circulating water and cooling to 40-60 DEG C, filtering off the materials, and drying and collecting a white powdered SMA resin with low molecular weight. The present invention uses an ''inverse suspension polymerization'' reaction mode, and uses the continuous evaporation reflux of the dispersed phase to control the reaction temperature and promptly discharge reaction heat, so that the reaction can be stably carried out. By controlling the ratio and dropping speed of monomer and initiator, and addition proportion of a chain transfer agent, the polymerization reaction can obtain a series of different molecular weights.
Description
Technical field
The present invention relates to the synthetic method field of lower molecular weight SMA resin, specifically, relate to a kind of synthetic method of papermaking printing lower molecular weight SMA resin.
Background technology
SMA resin is by the low-molecular-weight polymkeric substance of a class of vinylbenzene (styrene) same to maleic anhydride (MaleicAnhydride) block copolymerization.SMA base resin is white powder or sheet, can be dissolved in the aqueous solution of high pH value.SMA low-molecular-weight resin printing papermaking and letex polymerization industry in have widely with important purposes; Because vinylbenzene is very fast with the speed of response of maleic anhydride, and exothermic heat of reaction amount is large, and causes reacting and be difficult to control, easily cause molecular weight of copolymer distribute wide, product performance are unstable.In industrial production, by traditional polyreaction mode, be difficult to obtain value product.Foreign patent technique is " solvent polymeric " mainly, and aftertreatment technology is complicated, cost is high.The SMA low-molecular-weight resin of domestic use, the American-European import of main dependence, price is very high.
Summary of the invention
In order to overcome above-mentioned technical problem, the present invention discloses that a kind of range of molecular weight distributions is narrow, stable performance, the synthetic method of free of contamination low molecule SMA resin during production.
To achieve these goals, the synthetic method of a kind of lower molecular weight SMA resin of the present invention, comprises the following steps:
The first step: choose a certain amount of a, b and c tri-kinds of components as raw material, wherein, a component is monomer styrene, b component is the mixture that monomer maleic anhydride is dissolved in a solvent and is formed later, and c component is an initiator; Choose one with the reactor of A, B, C tri-tear drop tanks, in it, add a certain amount of dispersion agent and chain-transfer agent; A, b, c tri-kinds of components are added respectively in A tear drop tank, B tear drop tank and C tear drop tank;
Second step: the group in above-mentioned A tear drop tank, B tear drop tank and C tear drop tank at the uniform velocity drips in reactor after being heated to backflow by reactor respectively, and the stirring that remains a constant speed, drip used time 2-4 hour;
3rd step: after dropwising, continues to keep reflux state 1-2 hour, then passes into circulating water and filter discharging after 40-60 DEG C, the solid toluene cleaning 2-3 after filtration all over, dry and collect and obtain white powder low molecule SMA resin.
The synthetic method of a kind of low molecule SMA resin of the present invention, described solvent is butanone; Described initiator is BPO; Described chain-transfer agent is dodecyl base mercaptan; Wherein, according to mass ratio be: monomer styrene 260 parts, monomer maleic anhydride 80-260 part, BPO15-25 part, dodecyl base mercaptan 0.05-0.15 part, butanone 100-300 part, toluene 500-600 part.
The synthetic method of a kind of low molecule SMA resin of the present invention, described solvent is butanone; Described initiator is AIBN; Described chain-transfer agent is dodecyl base mercaptan; Wherein, according to mass ratio be: monomer styrene 260 parts, monomer maleic anhydride 80-260 part, AIBN15-25 part, dodecyl base mercaptan 0.05-0.15 part, butanone 100-300 part, toluene 500-600 part.
The synthetic method of a kind of low molecule SMA resin of the present invention, according to mass ratio, described monomer styrene is 170 parts, monomer maleic anhydride 250 parts, BPO20 part, 0.1 part, dodecyl base mercaptan, butanone 250 parts, toluene 550 parts.
The synthetic method of a kind of low molecule SMA resin of the present invention, according to mass ratio, described monomer styrene is 250 parts, monomer maleic anhydride 170 parts, AIBN20 part, 0.1 part, dodecyl base mercaptan, butanone 250 parts, toluene 550 parts.
The synthetic method of a kind of low molecule SMA resin of the present invention, the dropwise reaction time in second step is 3 hours.
The synthetic method of a kind of low molecule SMA resin of the present invention, described soaking time is 1.5 hours.
The present invention is the reactive mode using " Inverse suspension copolymerization ", with the continuous evaporation backflow of disperse phase, control temperature of reaction and drain reaction heat in time, reaction can be stablized carry out, by controlling proportioning and the rate of addition of monomer and initiator, and the additional proportion of chain-transfer agent, polyreaction obtains a series of different molecular weight, the product of different glass temperature, and be insoluble to disperse phase due to final product SMA resin, form pressed powder or a shape, dispersion or precipitation in a kettle., are easy to rear road process (filter, dry).With low cost, administration measure, technique easily realize industrialized mass production.
Embodiment
Embodiments of the invention are described below.The element described in one embodiment of the invention and feature can combine with the element shown in one or more other embodiments and feature.It should be noted that for purposes of clarity, in explanation, eliminate expression and the description of unrelated to the invention, parts known to persons of ordinary skill in the art or process.
Below the present invention is described further.
The synthetic method of a kind of low molecule SMA resin of the present invention, comprises the following steps:
Embodiment 1
The first step: choose a certain amount of a, b and c tri-kinds of components as raw material, wherein, a component is the monomer styrene of 260 parts, b component is the mixture that butanone that the monomer maleic anhydride of 85 parts is dissolved in 100 parts is formed later, and c component is the BPO of 10 parts; Choose one with the reactor of A, B, C tri-tear drop tanks, in it, add the toluene of 500 parts and the dodecyl base mercaptan of 0.05 part; A, b, c tri-kinds of components are added respectively in A tear drop tank, B tear drop tank and C tear drop tank;
Second step: the group in above-mentioned A tear drop tank, B tear drop tank and C tear drop tank at the uniform velocity drips in reactor after being heated to backflow by reactor respectively, and the stirring that remains a constant speed, drip 3 hours used times;
3rd step: after dropwising, continues to keep reflux state 2 hours, then passes into circulating water and filter discharging after 40-60 DEG C, the solid toluene after filtration clean 2 times, dry and collect and obtain white powder low molecule SMA resin.
Appearance character: white powdery solids
Acid number: 265
Second-order transition temperature: 115 degrees Celsius
Weight-average molecular weight: 10500
Embodiment 2
The first step: choose a certain amount of a, b and c tri-kinds of components as raw material, wherein, a component is the monomer styrene of 260 parts, b component is the mixture that butanone that the monomer maleic anhydride of 125 parts is dissolved in 150 parts is formed later, and c component is the BPO of 15 parts; Choose one with the reactor of A, B, C tri-tear drop tanks, in it, add the toluene of 500 parts and the dodecyl base mercaptan of 0.08 part; A, b, c tri-kinds of components are added respectively in A tear drop tank, B tear drop tank and C tear drop tank;
Second step: the group in above-mentioned A tear drop tank, B tear drop tank and C tear drop tank at the uniform velocity drips in reactor after being heated to backflow by reactor respectively, and the stirring that remains a constant speed, drip 3 hours used times;
3rd step: after dropwising, continues to keep reflux state 2 hours, then passes into circulating water and filter discharging after 40-60 DEG C, the solid toluene after filtration clean 2 times, dry and collect and obtain white powder low molecule SMA resin.
Appearance character: white powdery solids
Acid number: 335
Second-order transition temperature: 135 degrees Celsius
Weight-average molecular weight: 7500
Embodiment 3
The first step: choose a certain amount of a, b and c tri-kinds of components as raw material, wherein, a component is the monomer styrene of 260 parts, b component is the mixture that butanone that the monomer maleic anhydride of 250 parts is dissolved in 300 parts is formed later, and c component is the BPO of 25 parts; Choose one with the reactor of A, B, C tri-tear drop tanks, in it, add the toluene of 500 parts and the dodecyl base mercaptan of 0.15 part; A, b, c tri-kinds of components are added respectively in A tear drop tank, B tear drop tank and C tear drop tank;
Second step: the group in above-mentioned A tear drop tank, B tear drop tank and C tear drop tank at the uniform velocity drips in reactor after being heated to backflow by reactor respectively, and the stirring that remains a constant speed, drip 3 hours used times;
3rd step: after dropwising, continues to keep reflux state 2 hours, then passes into circulating water and filter discharging after 40-60 DEG C, the solid toluene after filtration clean 2 times, dry and collect and obtain white powder low molecule SMA resin.
Appearance character: white powdery solids
Acid number: 465
Second-order transition temperature: 155 degrees Celsius
Weight-average molecular weight: 5500
Embodiment 4
The first step: choose a certain amount of a, b and c tri-kinds of components as raw material, wherein, a component is the monomer styrene of 260 parts, b component is the mixture that butanone that the monomer maleic anhydride of 250 parts is dissolved in 300 parts is formed later, and c component is the AIBN of 22 parts; Choose one with the reactor of A, B, C tri-tear drop tanks, in it, add the toluene of 500 parts and the dodecyl base mercaptan of 0.15 part; A, b, c tri-kinds of components are added respectively in A tear drop tank, B tear drop tank and C tear drop tank;
Second step: the group in above-mentioned A tear drop tank, B tear drop tank and C tear drop tank at the uniform velocity drips in reactor after being heated to backflow by reactor respectively, and the stirring that remains a constant speed, drip 3 hours used times;
3rd step: after dropwising, continues to keep reflux state 2 hours, then passes into circulating water and filter discharging after 40-60 DEG C, the solid toluene after filtration clean 2 times, dry and collect and obtain white powder low molecule SMA resin.
Appearance character: white powdery solids
Acid number: 465
Second-order transition temperature: 155 degrees Celsius
Weight-average molecular weight: 5500
The present invention is the reactive mode using " Inverse suspension copolymerization ", with the continuous evaporation backflow of disperse phase, control temperature of reaction and drain reaction heat in time, reaction can be stablized carry out, by controlling proportioning and the rate of addition of monomer and initiator, and the additional proportion of chain-transfer agent, polyreaction obtains a series of different molecular weight, the product of different glass temperature, and be insoluble to disperse phase due to final product SMA resin, form pressed powder or a shape, dispersion or precipitation in a kettle., are easy to rear road process (filter, dry).With low cost, administration measure, technique easily realize industrialized mass production.
Although described the present invention and advantage thereof in detail, be to be understood that and can have carried out various change when not exceeding the spirit and scope of the present invention limited by appended claim, substituting and conversion.And the scope of the application is not limited only to the specific embodiment of process, equipment, means, method and step described by specification sheets.One of ordinary skilled in the art will readily appreciate that from disclosure of the present invention, can use perform the function substantially identical with corresponding embodiment described herein or obtain and its substantially identical result, existing and that will be developed in the future process, equipment, means, method or step according to the present invention.Therefore, appended claim is intended to comprise such process, equipment, means, method or step in their scope.
Claims (7)
1. a synthetic method for low molecule SMA resin, is characterized in that, comprises the following steps:
The first step: choose a certain amount of a, b and c tri-kinds of components as raw material, wherein, a component is monomer styrene, b component is the mixture that monomer maleic anhydride is dissolved in a solvent and is formed later, and c component is an initiator; Choose one with the reactor of A, B, C tri-tear drop tanks, in it, add a certain amount of dispersion agent and chain-transfer agent; A, b, c tri-kinds of components are added respectively in A tear drop tank, B tear drop tank and C tear drop tank;
Second step: the group in above-mentioned A tear drop tank, B tear drop tank and C tear drop tank at the uniform velocity drips in reactor after being heated to backflow by reactor respectively, and the stirring that remains a constant speed, drip used time 2-4 hour;
3rd step: after dropwising, continues to keep reflux state 1-2 hour, then passes into circulating water and filter discharging after 40-60 DEG C, the solid toluene cleaning 2-3 after filtration all over, dry and collect and obtain white powder low molecule SMA resin.
2. the synthetic method of low molecule SMA resin according to claim 1, is characterized in that, described solvent is butanone; Described initiator is BPO; Described chain-transfer agent is dodecyl base mercaptan; Wherein, according to mass ratio be: monomer styrene 260 parts, monomer maleic anhydride 80-260 part, BPO15-25 part, dodecyl base mercaptan 0.05-0.15 part, butanone 100-300 part, toluene 500-600 part.
3. the synthetic method of low molecule SMA resin according to claim 1, is characterized in that, described solvent is butanone; Described initiator is AIBN; Described chain-transfer agent is dodecyl base mercaptan; Wherein, according to mass ratio be: monomer styrene 260 parts, monomer maleic anhydride 80-260 part, AIBN15-25 part, dodecyl base mercaptan 0.05-0.15 part, butanone 100-300 part, toluene 500-600 part.
4. the synthetic method of low molecule SMA resin according to claim 2, it is characterized in that, according to mass ratio, described monomer styrene is 250 parts, monomer maleic anhydride 170 parts, BPO20 part, 0.1 part, dodecyl base mercaptan, butanone 250 parts, toluene 550 parts.
5. the synthetic method of low molecule SMA resin according to claim 3, it is characterized in that, according to mass ratio, described monomer styrene is 250 parts, monomer maleic anhydride 170 parts, AIBN20 part, 0.1 part, dodecyl base mercaptan, butanone 250 parts, toluene 550 parts.
6. the synthetic method of low molecule SMA resin according to claim 1, is characterized in that, the dropwise reaction time in second step is 3 hours.
7. the synthetic method of the low molecule SMA resin according to claim 1 or 6, is characterized in that, described soaking time is 1.5 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694554A (en) * | 2021-01-11 | 2021-04-23 | 浙江阿尔法化工科技有限公司 | Synthesis method and production equipment of SMA resin |
Citations (4)
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|---|---|---|---|---|
| CN101503490A (en) * | 2009-03-13 | 2009-08-12 | 北京化工大学 | Method for synthesizing low molecular weight phenylethylene / maleic anhydride alternate copolymer |
| CN101580564A (en) * | 2009-06-19 | 2009-11-18 | 北京化工大学 | Synthetic method of high molecular weight (HMW) alternating copolymer of styrene and maleic anhydride |
| CN102250273A (en) * | 2011-06-02 | 2011-11-23 | 北京化工大学 | Preparation method of styrene-maleic anhydride random copolymer |
| CN102653578A (en) * | 2011-03-04 | 2012-09-05 | 武陟县智辉化工有限责任公司 | Method for synthesizing styrene-maleic anhydride polymer through precipitation |
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2015
- 2015-08-12 CN CN201510493713.0A patent/CN105175598A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503490A (en) * | 2009-03-13 | 2009-08-12 | 北京化工大学 | Method for synthesizing low molecular weight phenylethylene / maleic anhydride alternate copolymer |
| CN101580564A (en) * | 2009-06-19 | 2009-11-18 | 北京化工大学 | Synthetic method of high molecular weight (HMW) alternating copolymer of styrene and maleic anhydride |
| CN102653578A (en) * | 2011-03-04 | 2012-09-05 | 武陟县智辉化工有限责任公司 | Method for synthesizing styrene-maleic anhydride polymer through precipitation |
| CN102250273A (en) * | 2011-06-02 | 2011-11-23 | 北京化工大学 | Preparation method of styrene-maleic anhydride random copolymer |
Non-Patent Citations (1)
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| 张国运: "SMA型表面施胶剂的制备与应用", 《造纸化学品》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694554A (en) * | 2021-01-11 | 2021-04-23 | 浙江阿尔法化工科技有限公司 | Synthesis method and production equipment of SMA resin |
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