CN104672409A - Research on synthetic condition of lignosulfonate modified polycarboxylate superplasticizer - Google Patents

Research on synthetic condition of lignosulfonate modified polycarboxylate superplasticizer Download PDF

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Publication number
CN104672409A
CN104672409A CN201310643569.5A CN201310643569A CN104672409A CN 104672409 A CN104672409 A CN 104672409A CN 201310643569 A CN201310643569 A CN 201310643569A CN 104672409 A CN104672409 A CN 104672409A
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China
Prior art keywords
reducer
modified polycarboxylate
water
lignin sulfonate
polycarboxylate water
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Pending
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CN201310643569.5A
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Chinese (zh)
Inventor
周相勇
许化强
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QINGDAO HUICHENG PETROCHEMICAL TECHNOLOGY Co Ltd
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QINGDAO HUICHENG PETROCHEMICAL TECHNOLOGY Co Ltd
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Priority to CN201310643569.5A priority Critical patent/CN104672409A/en
Publication of CN104672409A publication Critical patent/CN104672409A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a research on a synthetic condition of a lignosulfonate modified polycarboxylate superplasticizer. The research on the synthetic condition of the lignosulfonate modified polycarboxylate superplasticizer is characterized by being prepared by performing condensation on lignosulfonate, polyethylene glycol monomethyl ether metacrylic acid ester, acrylic acid and methacrylic acid sodium sulfonate in a ratio of (9-15 percent): (1-5 percent): (5-30 percent): (1-5 percent). An operation method comprises the following steps: mixing lignosulfonate, polyethylene glycol monomethyl ether metacrylic acid ester, acrylic acid and methacrylic acid sodium sulfonate in the ratio to prepare an aqueous solution with certain mass percentage (the mass percentage of water is 70-90 percent); preparing a diacetyl peroxide initiator into an aqueous solution and slowly dropwise adding the two solutions into a three-mouth flask by using a constant pressure dropping funnel; performing reaction for 2-10 hours at the temperature of 60-120 DEG C after the dropping is completed; cooling the system to be at room temperature after the reaction is completed, and regulating pH of the system to be 8-12 by using a sodium hydroxide solution to obtain the lignosulfonate modified polycarboxylate superplasticizer.

Description

A kind of synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer
Technical field
The present invention relates to a kind of synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer, belong to chemicals field.
Background of invention
Current poly carboxylic acid series water reducer, because of its higher water-reducing rate, fabulous slump-retaining and excellent reinforcing effect application and being widely used, has now received the favor of concrete works circle.The main raw material of poly carboxylic acid series water reducer derives from oil, and price is high, and does not belong to renewable resources.Sulfonated lignin are renewable, from the waste water in paper industry, and its low price, but water reducing ability is limited, can not meet the requirement of high performance concrete to water reducer.Have a lot of researchist that sulfonated lignin and poly carboxylic acid are carried out physical compounding, but directly composite water reducer effect affects very large by season, the cement place of production and adulterant item kind etc., water-reducing property is unsatisfactory.Few people carry out chemical modification to these 2 kinds of water reducers.
The present invention relates to a kind of synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer, under the condition being solvent with water, adopt free radical copolymerization method to synthesize lignin sulfonate modified polycarboxylate water-reducer.The water reducer that the present invention relates to not only can meet the requirement of high performance concrete to water reducer, and meets the requirement of current conservation-minded society.
Summary of the invention
A kind of synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer.
In order to achieve the above object, this invention takes following technical scheme:
The present invention relates to a kind of synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer, it is characterized in that:
Above-mentioned raw materials is preferably from paper mill byproduct sulfonated lignin.
Described raw material is: polyalkylene glycol acrylate monomethyl ether ester.
Described polymerization single polymerization monomer preferably from: one of vinylformic acid, methacrylic acid, methacrylic sulfonic acids sodium, butenoic acid or combination.
Described water is preferably from one of deionized water, distilled water, pure water.
Described initiator preferably from: one of hydrogen peroxide, diacetyl peroxide, dicumyl peroxide or combination.
Other reagent is preferred: sodium hydroxide.
The mass ratio of each component in system: ligninsulfonate: polyethylene glycol monomethyl ethermethacrylic acid esters: vinylformic acid: methacrylic sulfonic acids sodium is (9%-15%): (1-5%): (5-30%): (1-5%), and initiator amount accounts for the 1.5-5.0% of sulfonated lignin quality.
Concrete operation method: 2 kinds of solution constant pressure funnels are slowly instilled in there-necked flask after then initiator diacetyl peroxide being mixed with the aqueous solution equally by the aqueous solution (wherein the massfraction of water is 70-90%) above-mentioned ligninsulfonate, polyethylene glycol monomethyl ethermethacrylic acid esters, vinylformic acid and methacrylic sulfonic acids sodium being hybridly prepared into according to the above ratio certain mass mark.After being added dropwise to complete, under 60-120 DEG C of condition, react 2-10h.Having reacted rear cooling system to room temperature, is 8-12 with the pH of sodium hydroxide solution regulation system, can obtain the lignin sulfonate modified polycarboxylate water-reducer that patent of the present invention relates to.
Embodiment
Below in conjunction with embodiment, the present invention is described further, but is not limited only to this.
Embodiment 1:
Raw material and proportioning:
Ligninsulfonate: polyethylene glycol monomethyl ethermethacrylic acid esters: vinylformic acid: methacrylic sulfonic acids sodium is 9%:1%:5%:1%, and initiator amount accounts for 1.5% of sulfonated lignin quality.
Preparation method:
Concrete operation method: 2 kinds of solution constant pressure funnels are slowly instilled in there-necked flask after then initiator diacetyl peroxide being mixed with the aqueous solution equally by the aqueous solution (wherein the massfraction of water is 70-90%) above-mentioned ligninsulfonate, polyethylene glycol monomethyl ethermethacrylic acid esters, vinylformic acid and methacrylic sulfonic acids sodium being hybridly prepared into according to the above ratio certain mass mark.After being added dropwise to complete, under 60-120 DEG C of condition, react 2-10h.Having reacted rear cooling system to room temperature, is 8-12 with the pH of sodium hydroxide solution regulation system, can obtain the lignin sulfonate modified polycarboxylate water-reducer that patent of the present invention relates to.
Embodiment 2:
Raw material and proportioning:
Ligninsulfonate: polyethylene glycol monomethyl ethermethacrylic acid esters: vinylformic acid: methacrylic sulfonic acids sodium 12%:3%:20%:2%, initiator amount accounts for 2% of sulfonated lignin quality.
Concrete preparation method is with embodiment 1.
Embodiment 3:
Raw material and proportioning:
Ligninsulfonate: polyethylene glycol monomethyl ethermethacrylic acid esters: vinylformic acid: methacrylic sulfonic acids sodium 15%:5%:25%:5%, initiator amount accounts for 5.0% of sulfonated lignin quality.
Concrete preparation method is with embodiment 1.
Above-described embodiment is only and clearly the invention example is described, and the restriction not to the invention embodiment.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here exhaustive without the need to also giving all embodiments.

Claims (8)

1. the present invention relates to a kind of synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer, it is characterized in that described raw material preferably from paper mill byproduct sulfonated lignin and polyalkylene glycol acrylate monomethyl ether ester.
2. the synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer as claimed in claim 1, described polymerization single polymerization monomer is preferably from one of vinylformic acid, methacrylic acid, methacrylic sulfonic acids sodium, butenoic acid or combination.
3. the synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer as claimed in claim 1, described water is preferably from one of deionized water, distilled water, pure water.
4. lignin sulfonate modified polycarboxylate water-reducer as claimed in claim 1 synthesis condition research, described initiator preferably from: one of hydrogen peroxide, diacetyl peroxide, dicumyl peroxide or combination.
5. the synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer as claimed in claim 1, the preferred sodium hydroxide of other reagent.
6. the synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer as claimed in claim 1, temperature of reaction is 60-120 DEG C, and the reaction times is 2-10h, system pH is 8-12.
7. the synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer as claimed in claim 1, the mass ratio of each component in system: ligninsulfonate: polyethylene glycol monomethyl ethermethacrylic acid esters: vinylformic acid: methacrylic sulfonic acids sodium is (9%-15%): (1-5%): (5-30%): (1-5%), and initiator amount accounts for the 1.5-5.0% of sulfonated lignin quality.
8. the synthesis condition research of lignin sulfonate modified polycarboxylate water-reducer as claimed in claim 1, concrete operation method: 2 kinds of solution constant pressure funnels are slowly instilled in there-necked flask after then initiator diacetyl peroxide being mixed with the aqueous solution equally by the aqueous solution (wherein the massfraction of water is 70-90%) above-mentioned ligninsulfonate, polyethylene glycol monomethyl ethermethacrylic acid esters, vinylformic acid and methacrylic sulfonic acids sodium being hybridly prepared into according to the above ratio certain mass mark.After being added dropwise to complete, under 60-120 DEG C of condition, react 2-10h.Having reacted rear cooling system to room temperature, is 8-12 with the pH of sodium hydroxide solution regulation system, can obtain the lignin sulfonate modified polycarboxylate water-reducer that patent of the present invention relates to.
CN201310643569.5A 2013-12-03 2013-12-03 Research on synthetic condition of lignosulfonate modified polycarboxylate superplasticizer Pending CN104672409A (en)

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CN201310643569.5A CN104672409A (en) 2013-12-03 2013-12-03 Research on synthetic condition of lignosulfonate modified polycarboxylate superplasticizer

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106082754A (en) * 2016-06-24 2016-11-09 桂林华越环保科技有限公司 A kind of new concrete Light trabs early strength water-reducing agent
CN108996976A (en) * 2018-09-21 2018-12-14 成都市容德建筑劳务有限公司 Anti- slight crack preparation method of concrete

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106082754A (en) * 2016-06-24 2016-11-09 桂林华越环保科技有限公司 A kind of new concrete Light trabs early strength water-reducing agent
CN106082754B (en) * 2016-06-24 2018-05-22 桂林华越环保科技有限公司 A kind of concrete light wall panel early strength water-reducing agent
CN108996976A (en) * 2018-09-21 2018-12-14 成都市容德建筑劳务有限公司 Anti- slight crack preparation method of concrete

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Application publication date: 20150603