CN106279562B - A kind of synthesis technology of polycarboxylate water-reducer - Google Patents
A kind of synthesis technology of polycarboxylate water-reducer Download PDFInfo
- Publication number
- CN106279562B CN106279562B CN201610686774.3A CN201610686774A CN106279562B CN 106279562 B CN106279562 B CN 106279562B CN 201610686774 A CN201610686774 A CN 201610686774A CN 106279562 B CN106279562 B CN 106279562B
- Authority
- CN
- China
- Prior art keywords
- liquid
- water
- reducer
- polycarboxylate water
- reaction kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/1648—Porous product
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Structural Engineering (AREA)
- Chemically Coating (AREA)
Abstract
The synthesis technology of polycarboxylate water-reducer of the present invention, it is characterised in that: hydrogen peroxide is catalytically decomposed using P-Ti-Ni-Cr alloy, obtains the initiation oxygen atom that copolyreaction needs；Depositing formation on the agitating paddle of reaction kettle using electroless plating technology has nanometer level microporous spongy P-Ti-Ni-Cr alloy layer；The synthesis technology of polycarboxylate water-reducer: preparation A liquid；Prepare B liquid；In the reaction kettle equipped with electroless plating technology agitating paddle, the SPEG polymeric monomer of water, molecular weight 2400~2600 is added；It is added dropwise into reaction kettle by A liquid and B liquid；Sodium hydroxide and water are added into reaction kettle, polycarboxylate water-reducer product is made.The synthesis technology of polycarboxylate water-reducer of the present invention solves the problems, such as that production polycarboxylate water-reducer product is unstable under low temperature and room temperature, has the characteristics that energy conservation and environmental protection, reduces production cost in the case where not using reducing agent.
Description
Technical field
The present invention relates to chemical technology fields, belong to a kind of production method of polycarboxylate water-reducer, in particular to a kind of poly-
The synthesis technology of carboxylic acid water reducer.
Background technique
Water-reducing agent is most widely used a kind of additive in cement concrete production.Currently, the country is in the prior art
Polycarboxylate water-reducer is the third generation water-reducing agent product after calcium lignosulfonate and naphthalene water reducer.The polycarboxylate water-reducer root that tradition uses
It is divided into according to the initial temperature of production: three kinds of low temperature (0~15 DEG C), room temperature (20~30 DEG C), high temperature (40~60 DEG C) methods.With
Energy-saving and environment-friendly to require high temperature method production polycarboxylate water-reducer fewer and fewer, main cause is because being produced using high temperature method
Polycarboxylate water-reducer exists: the problems such as equipment investment is big, the production cycle is long, energy consumption is high.Low-temperature production process production polycarboxylic acids subtracts
Aqua is using oxidation -- and reduction system replaces the peroxide in high-temperature technology to decompose the initiation for obtaining copolyreaction at high temperature
Object oxygen atom, since the reaction speed of this reaction is affected by temperature greatly, because being influenced the starting temperature of production by seasonal variations temperature
Degree variation is very big, causes unstable product quality；It uses sulfites for reducing agent in production, produces sodium sulphate after reaction,
Cause to contain sodium sulphate in polycarboxylate water-reducer product produced, and purity is caused to reduce.
Summary of the invention
The present invention overcomes above-mentioned defects, it is therefore an objective to solve to produce polycarboxylate water-reducer under low temperature and room temperature
The unstable problem of product and energy conservation and environmental protection reduce production cost, provide a kind of synthesis technology of polycarboxylate water-reducer.
The synthesis technology content Description of polycarboxylate water-reducer of the present invention:
The synthesis technology of polycarboxylate water-reducer of the present invention, it is characterised in that: hydrogen peroxide is urged using P-Ti-Ni-Cr alloy
Change and decompose, obtains the initiation oxygen atom that copolyreaction needs；Formation is deposited on the agitating paddle of reaction kettle using electroless plating technology
With nanometer level microporous spongy P-Ti-Ni-Cr alloy layer；
The synthesis technology of polycarboxylate water-reducer:
(1), it prepares A liquid: being hybridly prepared into 150~200 ㎏ acrylic acid, 4~15 ㎏ mercaptopropionic acids, 50~100 ㎏ water
A liquid；
(2), it prepares B liquid: being hybridly prepared into B liquid with 5~20 ㎏ hydrogen peroxide, 150~200 ㎏ water；
(3), in the above-mentioned reaction kettle using electroless plating technology agitating paddle is installed, 1700 ㎏ water, molecular weight are added
2400~2,600 1000~2000 ㎏ of SPEG polymeric monomer；
(4), the speed that A liquid and B liquid were dripped off by 1.5~3 hours is added dropwise into reaction kettle, dropwise addition B liquid 5 first divides
Zhong Houzai starts that A liquid is added dropwise, and continues stirring after A drop adds 0.5~1 hour；
(5), 50 ㎏ sodium hydroxides and 1100 ㎏ water are added into reaction kettle, polycarboxylate water-reducer product is made.
The synthesis technology of polycarboxylate water-reducer of the present invention solves under low temperature and room temperature in the case where not using reducing agent
The unstable problem of polycarboxylate water-reducer product is produced, has the characteristics that energy conservation and environmental protection, reduces production cost.
Specific embodiment
The synthesis technology of polycarboxylate water-reducer of the present invention is achieved in that and illustrates below.
The present invention is catalytically decomposed hydrogen peroxide using P-Ti-Ni-Cr alloy, and it is former to obtain the initiation oxygen that copolyreaction needs
Son；The process is affected by temperature very little, and under identical hydrogen peroxide concentration and condition of different temperatures, the speed of production of oxygen atom is connect
Closely；
Depositing formation on the agitating paddle of reaction kettle using electroless plating technology has nanometer level microporous spongy P-Ti-
Ni-Cr alloy coating, P-Ti-Ni-Cr alloy layer is not required to before large area is damaged from new production in process of production.
The synthesis technology of polycarboxylate water-reducer of the present invention:
(1), it prepares A liquid: being hybridly prepared into 150~200 ㎏ acrylic acid, 4~15 ㎏ mercaptopropionic acids, 50~100 ㎏ water
A liquid；
(2), it prepares B liquid: being hybridly prepared into B liquid with 5~20 ㎏ hydrogen peroxide, 150~200 ㎏ water；
(3), in the above-mentioned reaction kettle using electroless plating technology agitating paddle is installed, 1700 ㎏ water, molecular weight are added
2400~2,600 1000~2000 ㎏ of SPEG polymeric monomer；
(4), the speed that A liquid and B liquid were dripped off by 1.5~3 hours is added dropwise into reaction kettle, dropwise addition B liquid 5 first divides
Zhong Houzai starts that A liquid is added dropwise, and continues heat preservation after A drop adds 0.5~1 hour；
(5), 50 ㎏ sodium hydroxides and 1100 ㎏ water are added into reaction kettle, polycarboxylate water-reducer product is made and is producing
Do not have to consider initial temperature in the process, obtained product is all identical.
The present invention is not influenced by season, and the product obtained under conditions of 0~40 DEG C of initial temperature is identical, improves production
The stability of product is not required to that reducing agent is added in production, has saved production cost.
Embodiment one
The synthesis technology of polycarboxylate water-reducer of the present invention is prepared under cryogenic:
(1), it under conditions of 3 DEG C of temperature, is sequentially added in the four-hole boiling flask with electroless plating technology agitating paddle: 170g
Water, 165g SPEG polymeric monomer, stirring to dissolution；
(2), A liquid is made into 20g acrylic acid, 1.25g mercaptopropionic acid, 20g water；
(3), B liquid is made into 2g hydrogen peroxide, 40g water；
(4), the speed that A liquid and B liquid were dripped off by 3 hours is added dropwise into four-hole boiling flask, is added dropwise B liquid 5 minutes first
Start that A liquid is added dropwise again afterwards, continues stirring 1 hour after A drop adds；
(5), 5g sodium hydroxide and 110g water are added into four-hole boiling flask, polycarboxylate water-reducer product is made.
Embodiment two
The synthesis technology of polycarboxylate water-reducer of the present invention is prepared under normal temperature conditions:
(1), it under conditions of 30 DEG C of temperature, is sequentially added in the four-hole boiling flask with electroless plating technology agitating paddle:
170g water, 165g SPEG polymeric monomer, stirring to dissolution；
(2), A liquid is made into 20g acrylic acid, 1.25g mercaptopropionic acid, 20g water；
(3), B liquid is made into 2g hydrogen peroxide, 40g water；
(4), the speed that A liquid and B liquid were dripped off by 3 hours is added dropwise into four-hole boiling flask, is added dropwise B liquid 5 minutes first
Start that A liquid is added dropwise again afterwards, continues stirring 1 hour after A drop adds；
(5), 5g sodium hydroxide and 110g water are added into four-hole boiling flask, polycarboxylate water-reducer product is made.
The polycarboxylate water-reducer that above-described embodiment one and embodiment two are obtained is by chemical examination detection, water-reducing rate, slump
Degree through when damage when it is essentially identical.
The synthesis technology of polycarboxylate water-reducer of the present invention, shadow of the initial temperature to product final performance when greatly reducing generation
It rings, solves the problems, such as that production polycarboxylate water-reducer product is unstable under low temperature and room temperature without using reducing agent,
Have the characteristics that energy conservation and environmental protection, reduces production cost.
Claims (3)
1. a kind of synthesis technology of polycarboxylate water-reducer, it is characterised in that: using P-Ti-Ni-Cr alloy to hydrogen peroxide catalysis point
Solution obtains the initiation oxygen atom that copolyreaction needs；Being deposited formation on the agitating paddle of reaction kettle using electroless plating technology is had
Nanometer level microporous spongy P-Ti-Ni-Cr alloy layer；
The synthesis technology of polycarboxylate water-reducer:
(1), it prepares A liquid: being hybridly prepared into A liquid with 150~200 ㎏ acrylic acid, 4~15 ㎏ mercaptopropionic acids, 50~100 ㎏ water；
(2), it prepares B liquid: being hybridly prepared into B liquid with 5~20 ㎏ hydrogen peroxide, 150~200 ㎏ water；
(3), in the above-mentioned reaction kettle using electroless plating technology agitating paddle is installed, 1700 ㎏ water of addition, molecular weight 2400~
2600 1000~2000 ㎏ of SPEG polymeric monomer；
(4), the speed that A liquid and B liquid were dripped off by 1.5~3 hours is added dropwise into reaction kettle, B liquid is added dropwise after five minutes first
Start that A liquid is added dropwise again, continues stirring after A drop adds 0.5~1 hour；
(5), 50 ㎏ sodium hydroxides and 1100 ㎏ water are added into reaction kettle, polycarboxylate water-reducer product is made.
2. the synthesis technology that one kind prepares polycarboxylate water-reducer under cryogenic, it is characterised in that: closed using P-Ti-Ni-Cr
Hydrogen peroxide is catalytically decomposed in gold, obtains the initiation oxygen atom that copolyreaction needs；Using electroless plating technology reaction kettle stirring
Deposition, which is formed, on paddle has nanometer level microporous spongy P-Ti-Ni-Cr alloy layer；
(1), it under conditions of 3 DEG C of temperature, is sequentially added in the four-hole boiling flask with electroless plating technology agitating paddle: 170g water,
165g SPEG polymeric monomer, stirring to dissolution；
(2), A liquid is made into 20g acrylic acid, 1.25g mercaptopropionic acid, 20g water；
(3), B liquid is made into 2g hydrogen peroxide, 40g water；
(4), the speed that A liquid and B liquid were dripped off by 3 hours is added dropwise into four-hole boiling flask, B liquid is added dropwise first after five minutes again
Start that A liquid is added dropwise, continues stirring 1 hour after A drop adds；
(5), 5g sodium hydroxide and 110g water are added into four-hole boiling flask, polycarboxylate water-reducer product is made.
3. the synthesis technology that one kind prepares polycarboxylate water-reducer under normal temperature conditions, it is characterised in that: closed using P-Ti-Ni-Cr
Hydrogen peroxide is catalytically decomposed in gold, obtains the initiation oxygen atom that copolyreaction needs；Using electroless plating technology reaction kettle stirring
Deposition, which is formed, on paddle has nanometer level microporous spongy P-Ti-Ni-Cr alloy layer；
(1), it under conditions of 30 DEG C of temperature, is sequentially added in the four-hole boiling flask with electroless plating technology agitating paddle: 170g water,
165g SPEG polymeric monomer, stirring to dissolution；
(2), A liquid is made into 20g acrylic acid, 1.25g mercaptopropionic acid, 20g water；
(3), B liquid is made into 2g hydrogen peroxide, 40g water；
(4), the speed that A liquid and B liquid were dripped off by 3 hours is added dropwise into four-hole boiling flask, B liquid is added dropwise first after five minutes again
Start that A liquid is added dropwise, continues stirring 1 hour after A drop adds；
(5), 5g sodium hydroxide and 110g water are added into four-hole boiling flask, polycarboxylate water-reducer product is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610686774.3A CN106279562B (en) | 2016-08-19 | 2016-08-19 | A kind of synthesis technology of polycarboxylate water-reducer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610686774.3A CN106279562B (en) | 2016-08-19 | 2016-08-19 | A kind of synthesis technology of polycarboxylate water-reducer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106279562A CN106279562A (en) | 2017-01-04 |
| CN106279562B true CN106279562B (en) | 2019-01-25 |
Family
ID=57660419
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610686774.3A Expired - Fee Related CN106279562B (en) | 2016-08-19 | 2016-08-19 | A kind of synthesis technology of polycarboxylate water-reducer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106279562B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4424320A (en) * | 1981-11-25 | 1984-01-03 | Phillips Petroleum Company | Polymerization with a silica base catalyst having titanium incorporated through use of peroxide |
| CN104513342A (en) * | 2015-01-12 | 2015-04-15 | 杭州绿怡新型建材有限公司 | Preparation method of normal temperature synthesized polycarboxylate superplasticizer |
-
2016
- 2016-08-19 CN CN201610686774.3A patent/CN106279562B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4424320A (en) * | 1981-11-25 | 1984-01-03 | Phillips Petroleum Company | Polymerization with a silica base catalyst having titanium incorporated through use of peroxide |
| CN104513342A (en) * | 2015-01-12 | 2015-04-15 | 杭州绿怡新型建材有限公司 | Preparation method of normal temperature synthesized polycarboxylate superplasticizer |
Non-Patent Citations (1)
| Title |
|---|
| "泡沫镍基体过氧化氢催化阴极";黄雯 等;《电源技术》;20130531;第137卷(第5期);767-769 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106279562A (en) | 2017-01-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105236798B (en) | A kind of preparation method of naphthalene water reducer | |
| CN1330600C (en) | Maleic acid anhydride series concrete water-reducing agent and preparation process thereof | |
| CN103739803B (en) | The synthetic method of imino-methyl-etherified aminoresin | |
| CN106431032B (en) | Microwave preparation method of α -calcium sulfate hemihydrate | |
| CN106517849A (en) | Oxidation-sulfonation starch water reducing agent preparation method | |
| CN104356316A (en) | Polycarboxylic acid water reducer prepared from running water and preparation method of polycarboxylic acid water reducer | |
| CN102951866A (en) | Ascorbic acid modified carboxylic water reducer and preparation method thereof | |
| CN101462842B (en) | Sulfonic acid ester retardation high efficiency water reducing agent and use thereof | |
| CN106279562B (en) | A kind of synthesis technology of polycarboxylate water-reducer | |
| CN102173635B (en) | Polycarboxylic acid high-slump-retaining zero-bleeding high-performance water reducing agent | |
| CN106830977B (en) | Production method for non-autoclaved self-insulation lightweight concrete building block | |
| CN110669212B (en) | Process for preparing metal-chelate retarder by using sol-gel method | |
| CN103601405A (en) | Aliphatic high-efficiency water reducing agent and preparation method thereof | |
| CN101659407A (en) | Thermal continuous synthesis method of lithium iron phosphate supercritical solvent | |
| CN109534712B (en) | Light yellow naphthalene water reducing agent and preparation method thereof | |
| CN111004362B (en) | Preparation method of naphthalene-based superplasticizer | |
| CN101734877A (en) | Method for preparing concrete high-efficiency water reducing agent by utilizing phenanthrene | |
| CN103275356A (en) | Method for preparing high-performance low-cobalt borate acylated cobalt adhesion promoter | |
| CN102408319A (en) | Production process of p-hydroxyanisole | |
| CN105347381A (en) | Preparing method of high purity calcium oxide | |
| CN105693948A (en) | Preparation method of green and environment-friendly, and high-stability polycarboxylic acid water reducing agent mother liquid | |
| CN107721832A (en) | A kind of preparation method of the fluorobenzene ether of 4 chlorine 3 | |
| CN204170727U (en) | A kind of preparation facilities of organic sodium alkoxide solution | |
| CN110330443B (en) | Synthetic process of p-chlorophenylhydrazine hydrochloride | |
| CN103483505A (en) | Polycarboxylate superplasticizer catalyzing production technology without high temperature |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190125 Termination date: 20210819 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |