CN109369904A - The performed polymer of the segment containing polyethenoxy ether and with the method for its polymeric monomer for preparing water-reducing agent - Google Patents
The performed polymer of the segment containing polyethenoxy ether and with the method for its polymeric monomer for preparing water-reducing agent Download PDFInfo
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- CN109369904A CN109369904A CN201811308549.1A CN201811308549A CN109369904A CN 109369904 A CN109369904 A CN 109369904A CN 201811308549 A CN201811308549 A CN 201811308549A CN 109369904 A CN109369904 A CN 109369904A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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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
- 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
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- 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)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Polyethers (AREA)
Abstract
The invention discloses a kind of performed polymer of segment containing polyethenoxy ether and with the method for its polymeric monomer for preparing water-reducing agent, performed polymer is the polymer that addition reaction acquisition is carried out by initiator ROH and propylene oxide, ethylene oxide, it includes the following steps: reaction kettle and pipeline carrying out Non-aqueous processing, vacuumize, and carries out inert gas purge after vacuumizing；Hold in reaction and initiator and catalyst mixing are added in kettle；It after progress temperature adjustment and will be maintained in reaction kettle, propylene oxide is added and be sequentially added into ethylene oxide progress ring-opening polymerization, and obtain performed polymer.The present invention improves the structure of polymeric monomer, synthesizes water-reducing agent with polymeric monomer prepared by the present invention by introducing polyethenoxy ether segment in performed polymer, absorption and shielding cement granules can preferably be played the role of, steric hindrance is enhanced, concrete guarantor's plasticity is more preferable, at low cost.
Description
Technical field
The present invention relates to water-reducing agent technical fields, and in particular to the performed polymer of the segment containing polyethenoxy ether and is subtracted with its preparation
The method of the polymeric monomer of aqua.
Background technique
Polymeric monomer is the most important raw material of polycarboxylate water-reducer, and the backbone of polymeric monomer provides powerful sky for water-reducing agent
Between steric hindrance.Domestic polycarboxylate water-reducer occupies absolute advantage, but large monomer technology innovation and development is slower.Inventor is to poly-
Carboxylic acid water reducer polymeric monomer has carried out a large amount of experimental study, discovery ingenious increase polyethenoxy ether in performed polymer, polymeric monomer
Segment and the control degree of polymerization can improve the structure of polycarboxylate water-reducer side chain, increase the steric hindrance effect of water-reducing agent and to cement
The absorption shielding action of particle is conducive to the diminishing dispersion performance and plasticity retentivity that improve synthesis water-reducing agent, and can basis
The diminishing of water-reducing agent protects plasticity requirements and adjusts polyethenoxy ether segment position and chain length.
Summary of the invention
The purpose of the present invention is introducing to polymerize short chain-polyethenoxy ether first in performed polymer, obtain containing polyoxypropylene
The performed polymer of ether segmented structure, has prepared a kind of novel polymeric monomer, and structure is more reasonable, it will preferably improves synthesis diminishing
The guarantor's plasticity and water-reducing rate of agent.
Technical scheme is as follows:
The invention discloses a kind of performed polymer of segment containing polyethenoxy ether for polymeric monomer, the performed polymer is by
Beginning agent ROH and propylene oxide carry out the polymer of addition reaction acquisition, the molecular structural formula of the polymer are as follows:
RO-(C3H60)x-H (1)
Wherein: x is the degree of polymerization of the polyethenoxy ether in structural formula (1), is 2~7 integer.
Further, the performed polymer is after initiator ROH and propylene oxide carry out addition reaction, with ethylene oxide
Carry out the polymer of addition reaction acquisition, the molecular structural formula of the polymer are as follows:
RO-(C3H60)x-(C2H4O)y-H (2)
Wherein: y is the degree of polymerization of polyoxyethylene ether in structural formula (2), is 1~7 integer.
Further, the performed polymer is the first and epoxy second before initiator ROH and propylene oxide carry out addition reaction
Alkane carries out the polymer of addition reaction acquisition, the molecular structural formula of the polymer are as follows:
RO-(C2H4O)z-(C3H60)x-H (3)
Wherein: z is the degree of polymerization of polyoxyethylene ether in structural formula (3), is 1~7 integer.
Further, the initiator is methallyl alcohol, prenol, glycol divinyl ether, propylene glycol vinyl
Any one in ether and 4- hydroxy butyl vinyl ether.
Further, the invention discloses a kind of method for preparing performed polymer, it includes the following steps:
Step 1: reaction kettle and pipeline are subjected to Non-aqueous processing, vacuumized, carries out inert gas purge after vacuumizing；
Step 2: holding in reaction and 1mol initiator be added in kettle, and catalyst mixing is added；
Step 3: controlling reactor temperature at 115~150 DEG C and maintain, and 2~7mol propylene oxide is added and is opened
Cyclopolymerization is reacted, and pressure control is in 0~0.45MPa in reaction kettle, until after pressure is constant in kettle, 15~30min of pressure stabilizing cools down
To 65~80 DEG C, performed polymer is obtained.
Further, be added in the step 3 propylene oxide and then it is secondary by reactor temperature control 100~
It 130 DEG C and maintains, 1~7mol ethylene oxide is added and carries out ring-opening polymerization, until after pressure is constant in kettle, pressure stabilizing 15~
30min。
Further, it is added before propylene oxide in the step 3, first controls reactor temperature 100~130
DEG C and maintain, be added 2~8mol ethylene oxide carry out ring-opening polymerization, until kettle in pressure it is constant after, pressure stabilizing 15~
30min。
Further, the catalyst is any one in sodium hydride, hydrofining, sodium methoxide, sodium ethoxide and potassium hydroxide
Kind.
Further, it is 0.06~0.12% that the catalyst for preparing performed polymer, which accounts for the weight ratio of performed polymer,.
Further, the invention discloses a kind of methods of polymeric monomer that water-reducing agent is prepared using performed polymer, it includes such as
Lower step:
Step 1: being added 1mol performed polymer in a kettle, and catalyst mixing is added；
Step 2: reactor temperature being controlled and at 100~130 DEG C and is maintained, be added 30~100mol ethylene oxide into
Row ring-opening polymerization, until 15~30min of pressure stabilizing is cooled to 65~80 DEG C, obtains polymeric monomer after pressure is constant in kettle.
Further, in the step 2 be added 30~100mol ethylene oxide after, successively into reaction kettle be added 2~
7mol propylene oxide and 20~70mol ethylene oxide carry out ring-opening polymerization, first will be in reaction kettle when propylene oxide is added
Temperature control is at 115~150 DEG C and maintains.
Further, in the step 2 be added 30~100mol ethylene oxide after, successively into reaction kettle be added 2~
It is poly- that 7mol propylene oxide, 30~100mol ethylene oxide, 2~7mol propylene oxide and 20~70mol ethylene oxide carry out open loop
Reaction is closed, first reactor temperature is controlled at 115~150 DEG C and maintained when propylene oxide is added.
Further, the catalyst for preparing polymeric monomer, which accounts for, is added the 0.06 of the sum of ethylene oxide and propylene oxide weight
~0.12%.
Performed polymer containing polyethenoxy ether segment of the invention and the polymeric monomer that water-reducing agent is prepared with it, feature is pre-polymerization
Polyethenoxy ether segment in body is close to the starting point of polymeric monomer, and the water-reducing agent of synthesis can enhance when leaning on close end and cement granules
Absorption or mutually absorption, have stronger adsorptivity and shield water molecular action to cement, are conducive to steric hindrance effect, than independent
Using the performed polymer of polyoxyethylene ether improve water-reducing agent guarantor's plasticity and cement slurry it is wrapped.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1
The invention discloses a kind of methods for preparing performed polymer comprising following steps:
Initiator methallyl alcohol 10mol (720g) is added in a kettle, catalyst sodium hydride 4.46g (material total amount
0.09%) mixing；Reactor temperature is controlled at 110 DEG C and maintained, ethylene oxide 80mol (3520g) is added and is opened
Cyclopolymerization is reacted, and pressure is controlled in 0~0.45MPa in reaction kettle, until after pressure is constant in kettle, 15~30min of pressure stabilizing；It will be anti-
Answer temperature in the kettle control at 130 DEG C and to maintain, be added propylene oxide 20mol (1160g), in reaction kettle pressure control 0~
0.45MPa, until 15~30min of pressure stabilizing is cooled to 65~80 DEG C, obtains performed polymer 5400g (molecule after pressure is constant in kettle
540) amount is.
The invention discloses a kind of methods of polymeric monomer that water-reducing agent is prepared using performed polymer comprising following steps:
Performed polymer 1mol (540g) is taken, catalyst sodium hydride 1.58g is added by 0.09% supplement of supplement inventory, it will be anti-
Temperature in the kettle control is answered at 110 DEG C and is maintained, ethylene oxide 30mol (1320g) is added and carries out ring-opening polymerization, until in kettle
After pressure is constant, 15~30min of pressure stabilizing is cooled to 65~80 DEG C, obtains the polymeric monomer A that number-average molecular weight is 18601, it is made big
After monomer, glacial acetic acid is added into reaction kettle, adjusting pH value is 5.5.
Wherein, general formula: n (amount of substance)=m (quality)/M (molal weight).
Embodiment 21
The invention discloses a kind of methods for preparing performed polymer comprising following steps:
Initiator prenol 10mol (860g) is added in a kettle, catalyst sodium methoxide 4.08g be (material total amount
0.08%) it mixes, reactor temperature is controlled at 115 DEG C and maintained, propylene oxide 20mol (1160g) is added and carries out open loop
Polymerization reaction, pressure control is in 0~0.45MPa in reaction kettle, until after pressure is constant in kettle, 15~30min of pressure stabilizing again will
Reactor temperature control at 105 DEG C and maintains, and is added ethylene oxide 70mol (3080g), in reaction kettle pressure control 0~
0.45MPa, until 15~30min of pressure stabilizing is cooled to 65~80 DEG C, obtains performed polymer 5100g (molecule after pressure is constant in kettle
510) amount is.
The invention discloses a kind of methods of polymeric monomer that water-reducing agent is prepared using performed polymer comprising following steps:
Performed polymer 1mol (510g) is taken, catalyst sodium hydride 4.06g is added by 0.08% supplement of supplement inventory；It will be anti-
Temperature in the kettle control is answered at 105 DEG C and is maintained, ethylene oxide 30mol (1760g) is added and carries out ring-opening polymerisation polymerization reaction, until
After pressure is constant in kettle, reactor temperature is controlled at 115 DEG C and is maintained again by 15~30min of pressure stabilizing, and propylene oxide is added
2mol (116g), until after pressure is constant in kettle, reactor temperature is controlled at 105 DEG C and tieed up again by 15~30min of pressure stabilizing
It holds, ethylene oxide 30mol (1760g) is added and carries out ring-opening polymerization, until after pressure is constant in kettle, 15~30min of pressure stabilizing,
Reactor temperature is controlled at 115 DEG C and maintained again, propylene oxide 2mol (116g) is added and carries out ring-opening polymerization, directly
After pressure is constant in kettle, reactor temperature is finally controlled at 105 DEG C and is maintained, is eventually adding ring by 15~30min of pressure stabilizing
Oxidative ethane 50mol (2900g) carries out polymerization reaction, until 15~30min of pressure stabilizing is cooled to 65~80 after pressure is constant in kettle
DEG C, obtain the polymeric monomer A that number-average molecular weight is 558221, after polymeric monomer is made, glacial acetic acid is added into reaction kettle, adjusts pH value
It is 7.
Initiator in the present invention be methallyl alcohol, prenol, glycol divinyl ether, propylene glycol vinyl ethers and
Any one in 4- hydroxy butyl vinyl ether, can be achieved good effect in the present invention；
Catalyst in the present invention refers to any one in sodium hydride, hydrofining, sodium methoxide, sodium ethoxide and potassium hydroxide
Kind, the weight ratio that the catalyst being added in preparing performed polymer accounts for performed polymer is 0.06~0.12%, is mended in preparing polymeric monomer
The catalyst filled, which accounts for, is added the 0.06~0.12% of the sum of ethylene oxide and propylene oxide weight, can be adjusted and be reacted according to its dosage
Temperature, charging rate can obtain same reaction effect.
It is not realistic to apply for example shown in table 1.
Examples 1 to 24 is to prepare performed polymer and polymeric monomer process control condition (being shown in Table 1)
Table 1:
Note:
M and n is illustrated respectively in the degree of polymerization that ethylene oxide and propylene oxide are added in the step of preparing polymeric monomer method two,
When 30~100mol ethylene oxide progress ring-opening polymerization is added, m1=30~100；
It is added after 30~100mol ethylene oxide in step 2,2~7mol propylene oxide is successively added into reaction kettle
When carrying out ring-opening polymerization with 20~70mol ethylene oxide, m1: n1: m2=30~100:2~7:20~70；
In step 2 be added 30~100mol ethylene oxide after, successively into reaction kettle be added 2~7mol propylene oxide,
When 30~100mol ethylene oxide, 2~7mol propylene oxide and 20~70mol ethylene oxide carry out ring-opening polymerization, m1: n1:
m2: n2: m3=30~100:2~7:20~70:2~7:20~70.
Each numerical value value range of m and n is in Examples 1 to 24.
Comparative example 1~7 is to prepare performed polymer and polymeric monomer process control condition (being shown in Table 2)
Table 2:
Polymeric monomer prepared by the present invention is used for chemical synthesis polycarboxylate water-reducer, carries out free radical using redox reaction
Copolymerization obtains polycarboxylate water-reducer (reference numeral is S-1~S-24), and its step are as follows:
300g water is added in reaction kettle, the polymeric monomer 350g in embodiment or comparative example is added, stirring is dissolved, and 4g is added
The mixed solution of 40g acrylic acid and 40g water is added dropwise with 120min, while 0.8g dimension is added dropwise with 150min for hydrogen peroxide (oxidant)
Mixed solution (the vinyl polyether monomer 45min drop of raw element C (reducing agent), 1.5g mercaptopropionic acid (chain-transferring agent) and 70g water
Add the mixed solution of 40g acrylic acid Yu 40g water, while 0.8g vitamin C, 1.5g mercaptopropionic acid and 70g water is added dropwise with 55min
Mixed solution).Reaction temperature is controlled at 5~40 DEG C, is dripped and is continued stirring curing heat preservation 60min, moisturizing is extremely into reaction kettle
1000g obtains colourless transparency liquid water-reducing agent.
The principle that redox system synthesizes polycarboxylate water-reducer is generated free radicals by redox reaction, in system
Oxidant species are first added, oxidant in reducing agent and solution is then added dropwise, redox reaction occurs, generate free radicals initiation
Monomer polymerization and synthesize water-reducing agent.
S-1~S-24 and comparative example 1~7 are prepared by the method polymeric monomer using the poly- carboxylic of redox system synthesis
The experiment characteristics table (being shown in Table 3) of sour water-reducing agent
Table 3:
Contain the short chain of polypropylene oxide in performed polymer of the invention, the polymeric monomer structure of preparation is more preferable, the diminishing of synthesis
Side chain can be made preferably to unfold in water in agent, from the performance comparison of above-described embodiment and reference examples as it can be seen that containing polyoxypropylene
The polymeric monomer of the performed polymer preparation of ether segment, polycarboxylate water-reducer flowing degree of net paste of cement (the cement paste initial flow of synthesis
240~287mm of degree) it is better than performed polymer corresponding polycarboxylate water-reducer (the cement paste initial flow of the pure polyoxyethylene ether of comparative example
230~271mm of dynamic degree), especially more prominent (the cement paste 60min fluidity of embodiment is 210~267mm to guarantor's plasticity, right
Ratio 60min fluidity is 195~230mm), play superior technique effect.
Above embodiment of the invention be only to clearly illustrate example of the present invention, and not be to this hair
The restriction of bright embodiment can also be done on the basis of the above description for those of ordinary skill in the art
Other various forms of variations or variation out here can not be exhaustive all embodiments, it is all belong to it is of the invention
The obvious changes or variations that technical solution is extended out are still in the scope of protection of the present invention.
Claims (13)
1. a kind of performed polymer of the segment containing polyethenoxy ether for polymeric monomer, which is characterized in that the performed polymer is by originating
Agent ROH and propylene oxide carry out the polymer of reaction acquisition, the molecular structural formula of the polymer are as follows:
RO-(C3H60)x-H (1)
Wherein: x is the degree of polymerization of the polyethenoxy ether in structural formula (1), is 2~7 integer.
2. the performed polymer of the segment according to claim 1 containing polyethenoxy ether for polymeric monomer, which is characterized in that described
Performed polymer is the polymer that reaction acquisition is carried out by initiator ROH, propylene oxide and ethylene oxide, the molecular structure of the polymer
Formula are as follows:
RO-(C3H60)x-(C2H4O)y-H (2)
Wherein: y is the degree of polymerization of polyoxyethylene ether in structural formula (2), is 1~7 integer.
3. the performed polymer of the segment according to claim 1 containing polyethenoxy ether for polymeric monomer, which is characterized in that described
Performed polymer is the polymer that reaction acquisition is carried out by initiator ROH, ethylene oxide and propylene oxide, the molecular structure of the polymer
Formula are as follows:
RO-(C2H4O)z-(C3H60)x-H (3)
Wherein: z is the degree of polymerization of polyoxyethylene ether in structural formula (3), is 1~7 integer.
4. the performed polymer of the segment containing polyethenoxy ether for polymeric monomer according to claims 1 to 3, which is characterized in that
The initiator ROH is methallyl alcohol, prenol, glycol divinyl ether, propylene glycol vinyl ethers and 4- hydroxyl butyl second
Any one in alkene ether.
5. a kind of method for preparing performed polymer as described in claim 1, which is characterized in that it includes the following steps:
Step 1: reaction kettle and pipeline are subjected to Non-aqueous processing, vacuumized, carries out inert gas purge after vacuumizing；
Step 2: holding in reaction and 1mol initiator be added in kettle, and catalyst mixing is added；
Step 3: controlling reactor temperature at 115~150 DEG C and maintain, and it is poly- that the progress open loop of 2~7mol propylene oxide is added
Reaction is closed, pressure control is in 0~0.45MPa in reaction kettle, until 15~30min of pressure stabilizing is cooled to 65 after pressure is constant in kettle
~80 DEG C, obtain performed polymer.
6. preparing the method for performed polymer according to claim 5, which is characterized in that in the step 3 be added propylene oxide it
Afterwards, reactor temperature is controlled at 100~130 DEG C and is maintained again, it is anti-that the progress ring-opening polymerisation of 1~7mol ethylene oxide is added
It answers, until after pressure is constant in kettle, 15~30min of pressure stabilizing.
7. preparing the method for performed polymer according to claim 5, which is characterized in that in the step 3 be added propylene oxide it
Before, first reactor temperature is controlled at 100~130 DEG C and maintained, it is anti-that the progress ring-opening polymerisation of 2~8mol ethylene oxide is added
It answers, until after pressure is constant in kettle, 15~30min of pressure stabilizing.
8. preparing the method for performed polymer according to claim 5, which is characterized in that the catalyst be sodium hydride, hydrofining,
Any one in sodium methoxide, sodium ethoxide and potassium hydroxide.
9. preparing the method for performed polymer according to claim 5, which is characterized in that the catalyst for preparing performed polymer accounts for pre-
The weight ratio of aggressiveness is 0.06~0.12%.
10. a kind of side for the polymeric monomer for preparing water-reducing agent using performed polymer described in any one of claim 5~7 claim
Method, which is characterized in that it includes the following steps:
Step 1: being added 1mol performed polymer in a kettle, and catalyst mixing is added；
Step 2: controlling reactor temperature at 100~130 DEG C and maintain, and 30~100mol ethylene oxide is added and is opened
Cyclopolymerization reaction, until 15~30min of pressure stabilizing is cooled to 65~80 DEG C, obtains polymeric monomer after pressure is constant in kettle.
11. the method that performed polymer prepares the polymeric monomer of water-reducing agent according to claim 10, which is characterized in that the step 2
After middle addition 30~100mol ethylene oxide, 2~7mol propylene oxide and 20~70mol epoxy are successively added into reaction kettle
Ethane carries out ring-opening polymerization, and first reactor temperature is controlled at 115~150 DEG C and maintained when propylene oxide is added.
12. the method that performed polymer prepares the polymeric monomer of water-reducing agent according to claim 10, which is characterized in that the step 2
After middle addition 30~100mol ethylene oxide, 2~7mol propylene oxide, 30~100mol epoxy are successively added into reaction kettle
Ethane, 2~7mol propylene oxide and 20~70mol ethylene oxide carry out ring-opening polymerization, first will when propylene oxide is added
Reactor temperature control is at 115~150 DEG C and maintains.
13. the method that performed polymer prepares the polymeric monomer of water-reducing agent according to claim 10, which is characterized in that the preparation is big
The catalyst of monomer, which accounts for, is added the 0.06~0.12% of the sum of ethylene oxide and propylene oxide weight.
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| EP1018530A2 (en) * | 1999-01-05 | 2000-07-12 | Kaneka Corporation | Method of producing reactive silicon group-containing polyether oligomers |
| CN102504239A (en) * | 2011-11-03 | 2012-06-20 | 山西合盛邦砼建材有限公司 | Catalyst for preparing polycarboxylate water reducing agent macromonomer and preparation method thereof |
| CN105330830A (en) * | 2014-08-15 | 2016-02-17 | 辽宁奥克化学股份有限公司 | Terminal alkenyl nonsaturated polyether and purpose thereof |
| CN108484897A (en) * | 2018-01-25 | 2018-09-04 | 北京砼帮汇科技有限公司 | A kind of polyoxy alkene ether monomer and the method for preparing polycarboxylate water-reducer with it |
-
2018
- 2018-11-05 CN CN201811308549.1A patent/CN109369904A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1018530A2 (en) * | 1999-01-05 | 2000-07-12 | Kaneka Corporation | Method of producing reactive silicon group-containing polyether oligomers |
| CN102504239A (en) * | 2011-11-03 | 2012-06-20 | 山西合盛邦砼建材有限公司 | Catalyst for preparing polycarboxylate water reducing agent macromonomer and preparation method thereof |
| CN105330830A (en) * | 2014-08-15 | 2016-02-17 | 辽宁奥克化学股份有限公司 | Terminal alkenyl nonsaturated polyether and purpose thereof |
| CN108484897A (en) * | 2018-01-25 | 2018-09-04 | 北京砼帮汇科技有限公司 | A kind of polyoxy alkene ether monomer and the method for preparing polycarboxylate water-reducer with it |
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Application publication date: 20190222 |