CN106966629A - A kind of preparation method of polycarboxylate superplasticizer mother liquor - Google Patents
A kind of preparation method of polycarboxylate superplasticizer mother liquor Download PDFInfo
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- CN106966629A CN106966629A CN201710237945.9A CN201710237945A CN106966629A CN 106966629 A CN106966629 A CN 106966629A CN 201710237945 A CN201710237945 A CN 201710237945A CN 106966629 A CN106966629 A CN 106966629A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of preparation method of polycarboxylate superplasticizer mother liquor, comprise the following steps：(1) unsaturated acids and water are made into the first solution；(2) oxidant and water are made into the second solution；(3) chain-transferring agent and the 3rd solution will be made into；(4) methacrylic polyoxyethylene ether, above-mentioned unsaturated acids, white sugar and water are added in reactor, regulation reaction temperature to 30~50 DEG C, stirring and dissolving；(5) the first solution, the second solution and the 3rd solution, 3~5h of time for adding, and the second solution is at the uniform velocity added dropwise simultaneously in the material obtained by step (4) and the 3rd late 10~30min of solution the first solution of ratio is dripped off；(6) after completion of dropwise addition, insulation reaction adds piece alkali and neutralized, produces polycarboxylic acids mother liquor；(7) above-mentioned polycarboxylic acids mother liquor and commercially available Point S08 diminishing mother liquors etc. are mixed containing solid 1: 1；(8) retarder, phosphate, sulfate and industrial production carbohydrate byproduct are added in the material obtained by step (7), it is well mixed to produce the polycarboxylate composite water reducing agent mother liquor.
Description
Technical field
The invention belongs to building material technical field, and in particular to a kind of preparation method of polycarboxylate superplasticizer mother liquor.
Background technology
In recent years, with the extensive development of China's infrastructure construction, the application of polycarboxylate water-reducer is more and more extensive.
Many advantages, such as polycarboxylate water-reducer has water-reducing rate high, little loss of slump and structure-controllable and as building neck in recent years
The focus of domain research.However, since 2015, the price straight rise of oxirane causes corresponding polyethers price
It is significantly increased, unit price rises to current 13000 yuan from initial 8000 yuan.Polyethers is to synthesize the larger one kind original of polycarboxylic acids demand
Material, jumping up for its price, greatly threatens the survival and development of concrete admixture industry.
On the other hand, with the development of modern industry, adjoint industry byproduct is seriously superfluous, and many enterprises itself can not
Complete digestion process, into dull material.This not only causes the significant wastage of resource, can also be caused to our living environment
Certain pollution.
Therefore, two methods are assembled and compound, while polycarboxylate water-reducer performance is increased, or polycarboxylate water-reducer
Under conditions of performance is constant, seeks a kind of preparation method for significantly reducing polycarboxylate water-reducer cost to concrete admixture, be
Existence to whole Concrete Industry is significant.
The content of the invention
It is an object of the invention to overcome prior art defect, there is provided a kind of preparation method of polycarboxylate superplasticizer mother liquor.
Technical scheme is as follows：
A kind of preparation method of polycarboxylate superplasticizer mother liquor, comprises the following steps：
(1) 8~21 parts by weight unsaturated acids and 20~30 parts by weight water are made into the first solution, the unsaturated acids is propylene
Acid and/or methacrylic acid；
(2) 0.5~1.3 parts by weight oxidant and 20~30 parts by weight water are made into the second solution；
(3) 0.4~1 parts by weight chain-transferring agent and 20~30 parts by weight water are made into the 3rd solution；
(4) by 198~200 parts by weight methacrylic polyoxyethylene ethers, the above-mentioned unsaturated acids of 1~4 parts by weight, 0.5
~2 parts by weight white sugar and 80~120 parts by weight water are added in reactor, regulation reaction temperature to 30~50 DEG C, stirring and dissolving；
(5) the first solution, the second solution and the 3rd solution is at the uniform velocity added dropwise simultaneously in the material obtained by step (4), is added dropwise
3~5h of time, and the second solution and the 3rd late 10~30min of solution the first solution of ratio drip off；
(6) after completion of dropwise addition, 1~2h of insulation reaction adds piece alkali and neutralized, produces polycarboxylic acids mother liquor；
(7) above-mentioned polycarboxylic acids mother liquor and commercially available Point-S08 diminishings mother liquor etc. are mixed containing solid 1: 1；
(8) in the material obtained by step (7) add 1~3% retarder, 0.5~1.5% phosphate, 0.5~
1.5% sulfate and 0.5~1.5% industrial production carbohydrate byproduct containing sugared ＞ 50%, it is well mixed to produce described gather
Carboxylic acid composite water-reducing agent mother liquor；Above-mentioned phosphate is biphosphate sodium hydrate, disodium hydrogen phosphate hydrate or tertiary sodium phosphate water
Compound, above-mentioned sulfate is alum, sodium pyrosulfite or thiosulfuric acid sodium hydrate.
In a preferred embodiment of the invention, the oxidant is hydrogen peroxide, ammonium persulfate or benzoyl peroxide first
Acyl.
In a preferred embodiment of the invention, the chain-transferring agent is mercaptoethanol, mercaptopropionic acid and hypophosphorous acid
At least one of sodium.
In a preferred embodiment of the invention, the mean molecule quantity of the methacrylic polyoxyethylene ether exists
2000~4800.
In a preferred embodiment of the invention, the retarder is white sugar, sodium gluconate or sodium citrate.
In a preferred embodiment of the invention, the industrial production carbohydrate byproduct is molasses or sodium gluconate
Byproduct.
Beneficial effects of the present invention：
1st, preparation method of the invention not only considerably reduces the production cost of polycarboxylic acids, will also be more industrial
Accessory substance is secondary to be utilized, and is not only increased the cost performance of polycarboxylic acids, is also reduced the waste and environmental pollution of industry byproduct.
2nd, preparation method production cost of the invention is relatively low, and production polyethers used is methacrylic polyoxyethylene ether
(HPEG) certain solid content, is instead of in reaction using white sugar, single ton of cost about reduces by 100 yuan, greatly reduces production
Cost.
3rd, preparation method of the invention has used relatively inexpensive chemical industry to produce accessory substance and food industry production pair
Product, with containing solid mother liquor, single ton of cost reduces by 500 yuan.Both the cost performance of polycarboxylic acids diminishing mother liquor had been improved, resource is reduced again
Waste and environment pollution.
4th, preparation method of the invention is without using special raw material, such as maleic anhydride or esters of acrylic acid, and it is synthesized
Products and marketing on existing product it is low compared to cost, water-reducing rate is high, and adaptability is good, especially in sandstone material preferably, market into
This relatively low Yunnan and Guangxi province have outstanding advantage, and can also solve construction well while production cost is reduced asks
Topic.
Embodiment
Technical scheme is further detailed and described below by way of embodiment.
Embodiment 1：
(1) 17 parts by weight of acrylic acid and 30 parts by weight water are made into the first solution；
(2) 1 parts by weight hydrogen peroxide and 30 parts by weight water are made into the second solution；
(3) 1 parts by weight mercaptoethanol and 30 parts by weight water are made into the 3rd solution；
(4) by 198 parts by weight methacrylic polyoxyethylene ethers (HPEG, mean molecule quantity 2000~4800), 3 weight
Part acrylic acid, 2 parts by weight white sugar and 100 parts by weight water are added in reactor, regulation reaction temperature to 50 DEG C, stirring and dissolving；
(5) the first solution, the second solution and the 3rd solution, first is at the uniform velocity added dropwise simultaneously in the material obtained by step (4)
The time for adding 3h of solution, and the second solution and the 3rd late 20min of solution the first solution of ratio drip off；
(6) after completion of dropwise addition, insulation reaction 1h adds 2 parts by weight piece alkali and neutralized, produces polycarboxylic acids mother liquor；
(7) above-mentioned polycarboxylic acids mother liquor and commercially available Point-S08 diminishings mother liquor etc. mix containing solid 1: 1 to (solid content is
35%)；
(8) white sugar of addition 2%, 0.5% biphosphate sodium hydrate, 1% Jiao in the material obtained by step (7)
Sodium sulfite and 1.5% molasses containing sugared ＞ 50%, it is well mixed to produce the polycarboxylate composite water reducing agent mother liquor.
Embodiment 2：
(1) 10 parts by weight of acrylic acid, 5 weight parts of methacrylic acid and 20 parts by weight water are made into the first solution；
(2) 0.5 parts by weight ammonium persulfate and 30 parts by weight water are made into the second solution；
(3) 1 parts by weight mercaptopropionic acid and 30 parts by weight water are made into the 3rd solution；
(4) by 200 parts by weight methacrylic polyoxyethylene ethers (HPEG, mean molecule quantity 2000~4800), 2 weight
Part acrylic acid, 1.5 parts by weight white sugar and 100 parts by weight water are added in reactor, regulation reaction temperature to 45 DEG C, stirring and dissolving；
(5) the first solution, the second solution and the 3rd solution, first is at the uniform velocity added dropwise simultaneously in the material obtained by step (4)
The time for adding 3h of solution, and the second solution and the 3rd late 30min of solution the first solution of ratio drip off；
(6) after completion of dropwise addition, insulation reaction 1h adds 4 parts by weight piece alkali and neutralized, produces polycarboxylic acids mother liquor；
(7) above-mentioned polycarboxylic acids mother liquor and commercially available Point-S08 diminishings mother liquor etc. mix containing solid 1: 1 to (solid content is
33%)；
(8) in the material obtained by step (7) add 3% sodium gluconate, 1% disodium hydrogen phosphate hydrate,
1.5% sodium thiosulfate and 1.5% molasses containing sugared ＞ 50%, it is well mixed to produce the polycarboxylate composite water reducing agent mother
Liquid.
Embodiment 3：
(1) 15 parts by weight of acrylic acid, 3 weight parts of methacrylic acid and 20 parts by weight water are made into the first solution；
(2) 0.5 parts by weight benzoyl peroxide and 30 parts by weight water are made into the second solution；
(3) 1 parts by weight sodium hypophosphite and 30 parts by weight water are made into the 3rd solution；
(4) by 200 parts by weight methacrylic polyoxyethylene ethers (HPEG, mean molecule quantity 2000~4800), 2 weight
Part acrylic acid, 1 parts by weight white sugar and 100 parts by weight water are added in reactor, regulation reaction temperature to 30 DEG C, stirring and dissolving；
(5) the first solution, the second solution and the 3rd solution, first is at the uniform velocity added dropwise simultaneously in the material obtained by step (4)
The time for adding 3h of solution, and the second solution and the 3rd late 30min of solution the first solution of ratio drip off；
(6) after completion of dropwise addition, insulation reaction 1h adds 6 parts by weight piece alkali and neutralized, produces polycarboxylic acids mother liquor；
(7) above-mentioned polycarboxylic acids mother liquor and commercially available Point-S08 diminishings mother liquor etc. mix containing solid 1: 1 to (solid content is
34%)；
(8) in the material obtained by step (7) add 3% sodium citrate, 1% tertiary sodium phosphate hydrate,
1% alum and the 1% sodium gluconate byproduct containing sugared ＞ 50%, it is well mixed to produce the polycarboxylate composite water reducing agent
Mother liquor.
Embodiment 4
The polycarboxylate composite water reducing agent mother liquor and comparative example that embodiment 1, embodiment 2,3 three kinds of schemes of embodiment are obtained
(commercially available Point-S08 diminishings mother liquor) compares, and using standard cement, volume presses cement quality 0.25%, according to GB8076-2008《It is mixed
Solidifying soil additive》, survey its concrete water-reducing ratio, the test concrete slump of solid volume 0.30% and through when slump-loss.
This experiment cement is southwestern cement PO.42.5, the Machine-made Sand of modulus of fineness 2.9~3.1；5~20mm continuous gradings are broken
Stone.Mixing time 120 seconds.Match ratio is：Cement 360kg/m3, blue or green sand 890kg/m3, yellow ground 210kg/m3, stone 800kg/m3,
Water 170kg/m3。
The foregoing is only a preferred embodiment of the present invention, therefore can not limit the scope that the present invention is implemented according to this, i.e.,
The equivalent changes and modifications made according to the scope of the claims of the present invention and description, all should still belong in the range of the present invention covers.
Claims (6)
1. a kind of preparation method of polycarboxylate superplasticizer mother liquor, it is characterised in that：Comprise the following steps：
(1) 8~21 parts by weight unsaturated acids and 20~30 parts by weight water are made into the first solution, the unsaturated acids is acrylic acid
And/or methacrylic acid；
(2) 0.5~1.3 parts by weight oxidant and 20~30 parts by weight water are made into the second solution；
(3) 0.4~1 parts by weight chain-transferring agent and 20~30 parts by weight water are made into the 3rd solution；
(4) by 198~200 parts by weight methacrylic polyoxyethylene ethers, the above-mentioned unsaturated acids of 1~4 parts by weight, 0.5~2 weight
Measure part white sugar and 80~120 parts by weight water are added in reactor, regulation reaction temperature to 30~50 DEG C, stirring and dissolving；
(5) the first solution, the second solution and the 3rd solution, time for adding 3 is at the uniform velocity added dropwise simultaneously in the material obtained by step (4)
~5h, and the second solution and the 3rd late 10~30min of solution the first solution of ratio drip off；
(6) after completion of dropwise addition, 1~2h of insulation reaction adds piece alkali and neutralized, produces polycarboxylic acids mother liquor；
(7) by above-mentioned polycarboxylic acids mother liquor and commercially available Point-S08 diminishings mother liquor etc. containing solid 1：1 mixing；
(8) retarder of addition 1~3%, 0.5~1.5% phosphate, 0.5~1.5% in the material obtained by step (7)
Sulfate and 0.5~1.5% industrial production carbohydrate byproduct containing sugared ＞ 50%, it is well mixed to produce the polycarboxylic acids and answer
Close water reducer mother liquor；Above-mentioned phosphate be biphosphate sodium hydrate, disodium hydrogen phosphate hydrate or tertiary sodium phosphate hydrate, on
Sulfate is stated for alum, sodium pyrosulfite or thiosulfuric acid sodium hydrate.
2. a kind of preparation method of polycarboxylate superplasticizer mother liquor as claimed in claim 1, it is characterised in that：The oxidant is
Hydrogen peroxide, ammonium persulfate or benzoyl peroxide.
3. a kind of preparation method of polycarboxylate superplasticizer mother liquor as claimed in claim 1, it is characterised in that：The chain-transferring agent
For at least one of mercaptoethanol, mercaptopropionic acid and sodium hypophosphite.
4. a kind of preparation method of polycarboxylate superplasticizer mother liquor as claimed in claim 1, it is characterised in that：The methallyl
The mean molecule quantity of base polyoxyethylene ether is 2000~4800.
5. a kind of preparation method of polycarboxylate superplasticizer mother liquor as claimed in claim 1, it is characterised in that：The retarder is
White sugar, sodium gluconate or sodium citrate.
6. a kind of preparation method of polycarboxylate superplasticizer mother liquor as claimed in claim 1, it is characterised in that：The industrial production
Carbohydrate byproduct is molasses or sodium gluconate byproduct.
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| CN201710237945.9A CN106966629A (en) | 2017-04-13 | 2017-04-13 | A kind of preparation method of polycarboxylate superplasticizer mother liquor |
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| CN201710237945.9A CN106966629A (en) | 2017-04-13 | 2017-04-13 | A kind of preparation method of polycarboxylate superplasticizer mother liquor |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708760A (en) * | 2013-12-23 | 2014-04-09 | 宁波中水科化工科技有限公司 | Slow-setting polycarboxylic acid water reducing agent and preparation method thereof |
| CN103964735A (en) * | 2014-05-04 | 2014-08-06 | 武汉华轩高新技术有限公司 | Preparation method for beet molasses-waste yeast liquid ultralow-hydration heat polycarboxylate water reducer |
| CN104261720A (en) * | 2014-09-22 | 2015-01-07 | 厦门天润锦龙建材有限公司 | Ether polycarboxylate superplasticizer and preparation method thereof |
| CN104761176A (en) * | 2015-03-31 | 2015-07-08 | 陕西友邦新材料科技有限公司 | Compound polycarboxylate superplasticizer and preparation method thereof |
-
2017
- 2017-04-13 CN CN201710237945.9A patent/CN106966629A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708760A (en) * | 2013-12-23 | 2014-04-09 | 宁波中水科化工科技有限公司 | Slow-setting polycarboxylic acid water reducing agent and preparation method thereof |
| CN103964735A (en) * | 2014-05-04 | 2014-08-06 | 武汉华轩高新技术有限公司 | Preparation method for beet molasses-waste yeast liquid ultralow-hydration heat polycarboxylate water reducer |
| CN104261720A (en) * | 2014-09-22 | 2015-01-07 | 厦门天润锦龙建材有限公司 | Ether polycarboxylate superplasticizer and preparation method thereof |
| CN104761176A (en) * | 2015-03-31 | 2015-07-08 | 陕西友邦新材料科技有限公司 | Compound polycarboxylate superplasticizer and preparation method thereof |
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Application publication date: 20170721 |