CN101143915A - Synthesis method for carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion - Google Patents
Synthesis method for carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion Download PDFInfo
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- CN101143915A CN101143915A CNA2007101443492A CN200710144349A CN101143915A CN 101143915 A CN101143915 A CN 101143915A CN A2007101443492 A CNA2007101443492 A CN A2007101443492A CN 200710144349 A CN200710144349 A CN 200710144349A CN 101143915 A CN101143915 A CN 101143915A
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- methyl methacrylate
- graft copolymer
- carboxymethyl cellulose
- copolymer emulsion
- methacrylate graft
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Abstract
The invention relates to a synthesis method of graft copolymer emulsion, in particular to a synthesis method of carboxymethylcellulose-methyl methacrylate graft copolymer emulsion. In the present method, surfactant needs to be added, as a result, cost is high, working procedures are many, and the prepared carboxymethylcellulose-methyl methacrylate graft copolymer cannot be used as additive for preparing plant fibre-inorganic matter composite materials; the invention resolves the problem. The synthesis method of the carboxymethylcellulose-methyl methacrylate graft copolymer emulsion of the invention includes two steps; firstly, sodium carboxymethylcellulose aqueous solution is heated and protected by inert gas; secondly, after the sodium carboxymethylcellulose aqueous solution is added with potassium persulphate and then methyl methacrylate, the carboxymethylcellulose-methyl methacrylate graft copolymer emulsion is obtained. The method of the invention does not need the surfactant, so cost is low, the process is simple, and the prepared carboxymethylcellulose-methyl methacrylate graft copolymer emulsion is suitable for preparing the plant fibre-inorganic matter composite materials.
Description
Technical field
The present invention relates to a kind of synthetic method of graft copolymer emulsion.
Background technology
The synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer has multiple, but in synthetic method in the past, all adopt organic solvent as dispersion medium, adopt cerium ammonium salt or azo class as initiator, and, must add tensio-active agent polyreaction is carried out smoothly because reaction is an inhomogeneous reaction; The cost height, but also to remove and reclaim organic solvent by processes such as filtration, distillation and dryings, operation is various, and can produce waste liquid, and environment is polluted.
In addition, method is in the past synthesized carboxymethyl cellulose-methyl methacrylate graft copolymer, because the polymerization degree of its grafted chain is all more than 100, the carboxymethyl cellulose-methyl methacrylate graft copolymer of preparing is particulate state, is difficult to be used to make vegetable fibre-inanimate matter problems of composite as additive.
Summary of the invention
The present invention is in the method that solves existing synthetic carboxymethyl cellulose-methyl methacrylate graft copolymer, need to add tensio-active agent, have the cost height, operation is various and the carboxymethyl cellulose-methyl methacrylate graft copolymer prepared is a particulate state, be difficult to use in the preparation problems of composite, and a kind of synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion is provided.
The carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion is synthetic as follows: be under the condition of 5～100r/min at 60～90 ℃, stirring velocity one,, Xylo-Mucine is dissolved in the water to form mass concentration be 2%～12% carboxymethyl cellulose aqueous solution, in reactor, feed the rare gas element evacuation of air, and keep protection of inert gas; Two, the Potassium Persulphate that adds Xylo-Mucine weight 1/30～1/15 after dissolving fully to Potassium Persulphate, adds the methyl methacrylate reaction 1.5～3.5 hours of 1/5～2 times of Xylo-Mucine weight again; Promptly obtain the carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion.
Rare gas element among the present invention is a kind of or wherein several mixture in nitrogen, helium, the argon gas.
The present invention adopts water as dispersion medium, adopt Potassium Persulphate as initiator, not only saved cost, and saved the treating processes of removing and reclaiming organic solvent, carboxymethyl cellulose is possess hydrophilic property not only, and have lipophilicity, and methyl methacrylate can be dissolved in reaction system well, do not need to add tensio-active agent.Compare with the vegetable fibre-inanimate matter matrix material auxiliary agent (for example milky white adhesive, isocyanate glue) of similar applications, synthetic carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion cost of the present invention has reduced by 50%～70%.The cost of carboxymethyl cellulose-methyl methacrylate graft copolymer per ton (in solid content 100%) is about 8500 yuan, and is similar to milky white adhesive, and the cost of isocyanate glue per ton up to 30,000 yuan about; Reaching under the situation of identical reinforced effects, the consumption of carboxymethyl cellulose-methyl methacrylate graft copolymer is a milky white adhesive 1/3rd, and is suitable with isocyanate glue, and visible product cost of the present invention is with the obvious advantage.
Synthetic carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion solid content of the present invention is 5%～20%, structure by fourier transform infrared spectroscopy mensuration, the proof methyl methacrylate successfully is grafted on the carboxymethyl cellulose, and the percentage of grafting of measuring methyl methacrylate by the energy dispersive x-ray analysis is 3～4.The polymerization degree of the carboxymethyl cellulose-methyl methacrylate graft copolymer grafted chain that the present invention makes is 2～8, is emulsion form, is suitable for being applied to the preparation of matrix material, is particularly useful for the preparation of various vegetable fibres-inanimate matter matrix material.
Description of drawings
Fig. 1 is the infrared spectrogram of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion.
Embodiment
Embodiment one: the carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion of present embodiment is synthetic as follows: be under the condition of 5～100r/min at 60～90 ℃, stirring velocity one,, Xylo-Mucine is dissolved in the water to form mass concentration be 2%～12% carboxymethyl cellulose aqueous solution, in reactor, feed the rare gas element evacuation of air, and keep protection of inert gas; Two, the Potassium Persulphate that adds Xylo-Mucine weight 1/30～1/15 after dissolving fully to Potassium Persulphate, adds the methyl methacrylate reaction 1.5～3.5 hours of 1/5～2 times of Xylo-Mucine weight again; Promptly obtain the carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion.
Embodiment two: the difference of present embodiment and embodiment one is: be under the condition of 20～80r/min Xylo-Mucine to be dissolved into that to form mass concentration in the water be 4%～10% carboxymethyl cellulose aqueous solution at 70～80 ℃, stirring velocity in the step 1.Other steps and parameter are identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment one is: be under the condition of 40～60r/min Xylo-Mucine to be dissolved into that to form mass concentration in the water be 6%～8% carboxymethyl cellulose aqueous solution at 72～78 ℃, stirring velocity in the step 1.Other steps and parameter are identical with embodiment one.
Embodiment four: the difference of present embodiment and embodiment one is: be under the condition of 50r/min Xylo-Mucine to be dissolved into that to form mass concentration in the water be 7% carboxymethyl cellulose aqueous solution at 75 ℃, stirring velocity in the step 1.Other steps and parameter are identical with embodiment one.
Embodiment five: the difference of present embodiment and embodiment one is: the Potassium Persulphate that adds Xylo-Mucine weight 1/25～1/20 in the step 2.Other steps and parameter are identical with embodiment one.
Embodiment six: the difference of present embodiment and embodiment one is: the Potassium Persulphate that adds Xylo-Mucine weight 1/22 in the step 2.Other steps and parameter are identical with embodiment one.
Embodiment seven: the difference of present embodiment and embodiment one is: the methyl methacrylate that adds 1/2～1.5 times of Xylo-Mucine weight in the step 2 again reacted 2～3 hours.Other steps and parameter are identical with embodiment one.
Embodiment eight: the difference of present embodiment and embodiment one is: the methyl methacrylate that adds 1.2 times of Xylo-Mucine weight in the step 2 again reacted 2.5 hours.Other steps and parameter are identical with embodiment one.
Embodiment nine: the difference of present embodiment and embodiment one is: the rare gas element in the step 1 is a kind of or wherein several combination in nitrogen, helium, the argon gas.Other steps and parameter are identical with embodiment one.
In the present embodiment when rare gas element be two kinds or two or more material when forming, press the arbitrary proportion mixing.
Embodiment ten: the carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion of present embodiment is synthetic as follows: be under the condition of 80r/min Xylo-Mucine to be dissolved into that to form mass concentration in the water be 10% carboxymethyl cellulose aqueous solution at 80 ℃, stirring velocity one,, in reactor, feed the nitrogen purge air, and keep nitrogen protection; Two, the Potassium Persulphate that adds Xylo-Mucine weight 1/25 after dissolving fully to Potassium Persulphate, adds the methyl methacrylate reaction 3 hours of Xylo-Mucine weight 1/2 again; Promptly obtain the carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion.
The percentage of grafting of the carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion that present embodiment makes is 4, and the grafted chain polymerization degree is 4.
Claims (9)
1. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion, it is characterized in that the carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion is synthetic as follows: be under the condition of 5～100r/min Xylo-Mucine to be dissolved into that to form mass concentration in the water be 2%～12% carboxymethyl cellulose aqueous solution one, at 60～90 ℃, stirring velocity, in reactor, feed the rare gas element evacuation of air, and keep protection of inert gas; Two, the Potassium Persulphate that adds Xylo-Mucine weight 1/30～1/15 after dissolving fully to Potassium Persulphate, adds the methyl methacrylate reaction 1.5～3.5 hours of 1/5～2 times of Xylo-Mucine weight again; Promptly obtain the carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion.
2. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion according to claim 1 is characterized in that in the step 1 at 70～80 ℃, stirring velocity being under the condition of 20～80r/min Xylo-Mucine to be dissolved into that to form mass concentration in the water be 4%～10% carboxymethyl cellulose aqueous solution.
3. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion according to claim 1 is characterized in that in the step 1 at 72～78 ℃, stirring velocity being under the condition of 40～60r/min Xylo-Mucine to be dissolved into that to form mass concentration in the water be 6%～8% carboxymethyl cellulose aqueous solution.
4. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion according to claim 1 is characterized in that in the step 1 at 75 ℃, stirring velocity being under the condition of 50r/min Xylo-Mucine to be dissolved into that to form mass concentration in the water be 7% carboxymethyl cellulose aqueous solution.
5. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion according to claim 1 is characterized in that in the step 2 adding the Potassium Persulphate of Xylo-Mucine weight 1/25～1/20.
6. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion according to claim 1 is characterized in that adding the Potassium Persulphate of Xylo-Mucine weight 1/22.
7. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion according to claim 1 is characterized in that the methyl methacrylate that adds 1/2～1.5 times of Xylo-Mucine weight in the step 2 again reacted 2～3 hours.
8. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion according to claim 1 is characterized in that the methyl methacrylate that adds 1.2 times of Xylo-Mucine weight in the step 2 again reacted 2.5 hours.
9. the synthetic method of carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion according to claim 1 is characterized in that rare gas element in the step 1 is a kind of or wherein several combination in nitrogen, helium, the argon gas.
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| CNA2007101443492A CN101143915A (en) | 2007-09-21 | 2007-09-21 | Synthesis method for carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion |
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| CNA2007101443492A CN101143915A (en) | 2007-09-21 | 2007-09-21 | Synthesis method for carboxymethyl cellulose-methyl methacrylate graft copolymer emulsion |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831033A (en) * | 2010-05-19 | 2010-09-15 | 西南科技大学 | Method for preparing environment-friendly modified carboxymethyl cellulose thermoplastic material |
| CN102558447A (en) * | 2012-01-13 | 2012-07-11 | 西北师范大学 | Carboxymethyl cellulose grafted copolymer emulsion for humidity-adjusting coating and preparation method thereof |
| CN106366384A (en) * | 2016-08-30 | 2017-02-01 | 安徽蓝德集团股份有限公司 | High-tenacity power cable sheathing compound |
| CN106749926A (en) * | 2016-11-30 | 2017-05-31 | 东北林业大学 | Improve the additive and its preparation and application of cement mortar bending and compressive strength |
| CN108892751A (en) * | 2018-06-05 | 2018-11-27 | 江南大学 | A kind of preparation method and application of sodium carboxymethylcellulose-ketene dimer graft copolymer |
| CN110747454A (en) * | 2019-11-19 | 2020-02-04 | 安徽鑫发铝业有限公司 | Production method of aluminum profile for air purifier shell |
-
2007
- 2007-09-21 CN CNA2007101443492A patent/CN101143915A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831033A (en) * | 2010-05-19 | 2010-09-15 | 西南科技大学 | Method for preparing environment-friendly modified carboxymethyl cellulose thermoplastic material |
| CN101831033B (en) * | 2010-05-19 | 2012-08-08 | 西南科技大学 | Method for preparing environment-friendly modified carboxymethyl cellulose thermoplastic material |
| CN102558447A (en) * | 2012-01-13 | 2012-07-11 | 西北师范大学 | Carboxymethyl cellulose grafted copolymer emulsion for humidity-adjusting coating and preparation method thereof |
| CN106366384A (en) * | 2016-08-30 | 2017-02-01 | 安徽蓝德集团股份有限公司 | High-tenacity power cable sheathing compound |
| CN106749926A (en) * | 2016-11-30 | 2017-05-31 | 东北林业大学 | Improve the additive and its preparation and application of cement mortar bending and compressive strength |
| CN106749926B (en) * | 2016-11-30 | 2018-09-14 | 东北林业大学 | Improve the additive and its preparation and application of cement mortar bending and compressive strength |
| CN108892751A (en) * | 2018-06-05 | 2018-11-27 | 江南大学 | A kind of preparation method and application of sodium carboxymethylcellulose-ketene dimer graft copolymer |
| CN108892751B (en) * | 2018-06-05 | 2020-11-27 | 江南大学 | Preparation method and application of sodium carboxymethylcellulose-diketene graft copolymer |
| CN110747454A (en) * | 2019-11-19 | 2020-02-04 | 安徽鑫发铝业有限公司 | Production method of aluminum profile for air purifier shell |
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