CN106278962A - A kind of methylacryoyloxyethyl dimethyl propylene ichthyodin and preparation method thereof - Google Patents
A kind of methylacryoyloxyethyl dimethyl propylene ichthyodin and preparation method thereof Download PDFInfo
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- CN106278962A CN106278962A CN201610674542.6A CN201610674542A CN106278962A CN 106278962 A CN106278962 A CN 106278962A CN 201610674542 A CN201610674542 A CN 201610674542A CN 106278962 A CN106278962 A CN 106278962A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
- C07C309/01—Sulfonic acids
- C07C309/02—Sulfonic acids having sulfo groups bound to acyclic carbon atoms
- C07C309/03—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
- C07C309/13—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton
- C07C309/14—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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Abstract
The invention discloses a kind of methylacryoyloxyethyl dimethyl propylene ichthyodin and preparation method thereof, disclose methylacryoyloxyethyl dimethyl propylene ichthyodin molecular structure；The preparation method of methylacryoyloxyethyl dimethyl propylene ichthyodin is disclosed simultaneously: first weigh the 1 of different amounts, 3 propyl sulfonic acid internal ester monomer and N, N dimethylaminoethyl methacrylate monomer, use different feed way, 1 will prepared in advance, 3 propyl sulfonic acid internal ester monomer acetone solns and N, N dimethylaminoethyl methacrylate monomer acetone soln join in round-bottomed flask, lucifuge single step reaction certain time；Ice-water bath cooling, sucking filtration, it is vacuum dried to obtain finished product.The present invention is respectively provided with splendid dispersive property, superior guarantor's plasticity energy and higher epistasis energy morning to cement system or concrete；Meanwhile, the potential hazard in armored concrete, steel bar corrosion brought can also be eliminated.
Description
Technical field
The invention belongs to the synthesis technical field of high performance water reducing agent of polyocarboxy acid both sexes organic active monomer, particularly relate to one
Plant the methacryloxypropyl second for synthesizing the both sexes organic active monomer without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid
Base dimethyl propylene ichthyodin and preparation method thereof.
Background technology
Along with country's " one with a road " implementation and the foundation of Asia infrastructure investment bank, public affairs will be accelerated
The construction of the large projects such as road, bridge, railway, dam, ocean, harbour and nuclear power.Modern concrete structure depends on height
Performance concrete technology, high performance concrete is extensive with its raw material sources, cheap, preparation technology simple and intensity is higher by one
Directly it is widely used in foundation construction field.High performance concrete has become Asia or even World Modern infrastructure concrete works
The construction material that consumption is maximum, China's high performance concrete yield has accounted for more than the 70% of world's consumption.Poly-carboxylic high-performance
Water reducer is one of key foundation realizing technology of high performance concrete.Current commercially available poly carboxylic acid series water reducer, still exist from
Scattered property is big, diminishing is poor, the defects such as damage is big and the lowest of collapsing, it is difficult to meet the requirement of high-performance, ultra-high performance concrete.Therefore,
Develop a series of a new generations high performance water reducing agent of polyocarboxy acid extremely urgent.Wherein, have because of amphoteric high performance water reducing agent of polyocarboxy acid
The distinguishing features such as low-dosage, high dispersive, low damage of collapsing, high diminishing and height are the strongest are had to enjoy countries in the world association area experts and scholars
Concern and attention.
So-called amphoteric high performance water reducing agent of polyocarboxy acid, is that one has pectinate texture, carries on its molecular backbone simultaneously
There is the amphiphilic polymers of zwitterion group.Amphoteric high performance water reducing agent of polyocarboxy acid both shown low-dosage, high diminishing excellent
Elegant performance, shows again splendid dispersive property, superior function of slump protection and higher epistasis energy morning, by Germany Johann
Doctor Plank is divided into forth generation polycarboxylic acid series high efficiency water reducing agent.Amphoteric high performance water reducing agent of polyocarboxy acid why have as
This excellent properties,
Mainly by improving what water reducer adsorbance was realized by cement essential mineral.Cement essential mineral composition is silicic acid three
Calcium (C3S), dicalcium silicate (C2S), tricalcium aluminate (C3And tetra calcium aluminoferrite (C A)4AF), wherein C3S、C2S is electronegative, C3A、C4AF
How positively charged, improve cement essential mineral to water reducer adsorbance, if an important thinking is exactly can be water reducer molecule master
Introduce cation organic active group on chain, at this moment, cement essential mineral composition C can be improved3S、C2The S adsorbance to water reducer,
Thus improve the cement system mineral composition total adsorbance to water reducer, to improve the combination property of concrete.At present, diminishing
Agent to introduce cation organic active group on its molecular backbone, is by adding the activated monomer Han quaternary ammonium salt cationic mostly
As MAPTAC, DMDAAC, DMC, CAC etc. realize., these activated monomers Han quaternary ammonium salt cationic are in uniform temperature
Under, add a certain amount of polymerization inhibitor, be prepared from by multistep reaction under a certain amount of initiator initiation.It is prepared
Cost height, complicated process of preparation, poor controllability, and, the equal chloride ion-containing of these activated monomers Han quaternary ammonium salt cationic, easily make
Become steel bar corrosion.With the activated monomer containing quaternary ammonium salt cationic such as MAPTAC, DMDAAC, DMC, CAC as raw material, anti-by polymerization
Should, amphoteric polycarboxylate water-reducer can be synthesized, if the amphoteric polycarboxylate water-reducer of these types to be used for armored concrete knot
In structure engineering, deduction and exemption bring potentially hazardous.
Summary of the invention
It is an object of the invention to provide a kind of methylacryoyloxyethyl dimethyl propylene ichthyodin and preparation method thereof, purport
Solving current quaternary ammonium salt cationic activated monomer preparation cost height, complicated process of preparation, the problem of poor controllability.
The present invention is achieved in that a kind of methylacryoyloxyethyl dimethyl propylene ichthyodin, this methacryloxypropyl
Ethyl dimethyl propylene ichthyodin molecular structure is:
。
The preparation method of a kind of methylacryoyloxyethyl dimethyl propylene ichthyodin comprises the following steps:
First the 1 of different amounts is weighed, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer,
Being dissolved separately in compound concentration in the acetone reaction dissolvent of 40mL is 1.125～1.875mol L-11,3-propyl sulfonic acid in
Ester monomer acetone soln and N, N-dimethylaminoethyl methacrylate monomer acetone soln；
Use different feed way, 1 will prepared in advance, 3-propyl sulfonic acid internal ester monomer acetone soln and N, N-dimethylamino
Ethyl methacrylate monomer acetone soln joins in round-bottomed flask, sealing, at 25 DEG C, and lucifuge single step reaction one timing
Between；
Reaction end is placed on frozen water bath and cools down, and separates out product and is placed on pressure-reduction filter device sucking filtration, then through low temperature (-
10 DEG C～10 DEG C) after washing with acetone 3 times, then at 25 DEG C, it is vacuum dried 24h, obtain a kind of for synthesizing without chloride ion amphoteric
The both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin finished product of high performance water reducing agent of polyocarboxy acid.
Further, described 1,3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer molar
Ratio is 0.75～1.25: 1.
Further, described different feed way is: with acetone reaction dissolvent for end liquid, be sequentially added into N, N-dimethylamino
Ethyl methacrylate monomer and 1,3-propyl sulfonic acid internal ester monomer；It is initially charged N, N-dimethylaminoethyl methacrylate list
Body acetone soln is slowly added dropwise 1,3-propyl sulfonic acid internal ester monomer acetone soln again；Or it is initially charged 1,3-propyl sulfonic acid lactone list
Body acetone soln is slowly added dropwise N, N-dimethylaminoethyl methacrylate monomer acetone soln again.
Further, described at 25 DEG C the lucifuge single step reaction time be 36 h～60h.
Methylacryoyloxyethyl dimethyl propylene ichthyodin that the present invention provides and preparation method thereof, synthesizes by the above process
A kind of for synthesizing the both sexes organic active monomer methacryloxypropyl without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid
Ethyl dimethyl propylene ichthyodin, this kind is for synthesizing the both sexes organic active without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid
Monomer methylacryoyloxyethyl dimethyl propylene ichthyodin, its productivity is up to more than 92.6%；With this kind of both sexes organic active list
Body methylacryoyloxyethyl dimethyl propylene ichthyodin, acrylic acid and monomethyl polyethylene glycol acrylate ester macromonomer are main
Want reaction raw materials, under strong oxidizer effect, by redox reaction, synthesized at normal temperatures without the poly-carboxylic of chloride ion amphoteric
Acid high-performance water reducing agent, is that 0.20%(is to account in terms of cement quality mark at its addition) time, cement paste initial flow degree exists
More than 325mm, after standing 90min, fluidity is maintained at more than 315mm, and concrete water-reducing ratio, up to more than 41%, initially collapses
Degree slump after more than 235mm, 90min stills remain in more than 220mm, 3d and 28d curing age concrete crushing strength
Ratio is respectively at 205% and more than 160% (the cement paste ratio of mudm w/m c=0.29, flowing degree of net paste of cement is with reference to national standard
" Methods for testing uniformity of concrete admixture " (GB/T 8077-2012) measures；C50 concrete mix is:m (Binder Materials)∶m (sand)∶m (stone)∶m (water)=450: 745: 1165: 144, concrete water-reducing ratio and mixture slump reference national standard are " outside concrete
Add agent " (GB/T 8076-2008) and " Standard for test methods of properties of ordinary concrete mixture standard " (GB/T 50080-2002)
Testing, compressive strength rate is with reference to national standard " standard for test methods of mechanical properties of ordinary concrete " (GB/T 50081-
2002) test).
The present invention is at 25 DEG C, uses and is initially charged N, N-dimethylaminoethyl methacrylate monomer acetone soln again
Being slowly added dropwise 1, the feed way of 3-propyl sulfonic acid internal ester monomer acetone soln, by selecting reasonable reaction monomer consumption and
The step response time is prepared from, and it is except, in addition to playing a role in terms of reducing cost, Simplified flowsheet, also having the spy of high yield
Point；And using finished product of the present invention as dominant response raw material, at normal temperatures by made by redox reaction without chloride ion
Amphoteric high performance water reducing agent of polyocarboxy acid, compared with commercial anionic type polycarboxylate water-reducer, in the case of volume is relatively low, right
Cement system or concrete are respectively provided with splendid dispersive property, superior guarantor's plasticity energy and higher epistasis energy morning；Meanwhile, also may be used
Eliminate the potential hazard in armored concrete, steel bar corrosion brought.
Accompanying drawing explanation
Fig. 1 is the preparation method flow process of the methylacryoyloxyethyl dimethyl propylene ichthyodin that the embodiment of the present invention provides
Figure.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, to the present invention
It is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to
Limit the present invention.
Below in conjunction with the accompanying drawings the application principle of the present invention is further described.
A kind of methylacryoyloxyethyl dimethyl propylene ichthyodin that the present invention provides, this methylacryoyloxyethyl diformazan
Base propane sulfonic acid ammonium molecular structure is:
。
As shown in Figure 1: the preparation method bag of a kind of methylacryoyloxyethyl dimethyl propylene ichthyodin that the present invention provides
Include following steps:
S101: first weigh 1,3-propyl sulfonic acid internal ester monomer and N, the N-dimethylaminoethyl methacrylate of different amounts
Monomer, being dissolved separately in compound concentration in the acetone reaction dissolvent of 40mL is 1.125～1.875mol L-11,3-propyl group sulphur
Acid lactone monomer acetone soln and N, N-dimethylaminoethyl methacrylate monomer acetone soln；
S102: use different feed way, 1 will prepared in advance, 3-propyl sulfonic acid internal ester monomer acetone soln and N, N-bis-
Methyaminomethyl acrylic acid ethyl ester monomer acetone soln joins in round-bottomed flask, sealing, at 25 DEG C, and lucifuge single step reaction one
Fix time；
S103: reaction end is placed on frozen water bath and cools down, separates out product and is placed on pressure-reduction filter device sucking filtration, then through low
After the washing with acetone of temperature-10 DEG C～10 DEG C 3 times, then at 25 DEG C, it is vacuum dried 24h, obtains a kind of for synthesizing without chloride ion two
The both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin finished product of property type high performance water reducing agent of polyocarboxy acid.
Further, described 1,3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer molar
Ratio is 0.75～1.25: 1.
Further, described different feed way is: with acetone reaction dissolvent for end liquid, be sequentially added into N, N-dimethylamino
Ethyl methacrylate monomer and 1,3-propyl sulfonic acid internal ester monomer；It is initially charged N, N-dimethylaminoethyl methacrylate list
Body acetone soln is slowly added dropwise 1,3-propyl sulfonic acid internal ester monomer acetone soln again；Or it is initially charged 1,3-propyl sulfonic acid lactone list
Body acetone soln is slowly added dropwise N, N-dimethylaminoethyl methacrylate monomer acetone soln again.
Further, described at 25 DEG C the lucifuge single step reaction time be 36 h～60h.
It is an object of the invention to provide a kind of for synthesizing the both sexes without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid
Organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin；The abundant raw material source used during preparation, price is just
Preferably, preparation technology is relatively easy.With obtained both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin,
Acrylic acid and monomethyl polyethylene glycol acrylate ester macromonomer are primary raw material, under strong oxidizer effect, by oxidation
Reduction reaction, can prepare at normal temperatures without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid, and this water reducer is relatively low at volume
In the case of there is the features such as splendid dispersive property, superior guarantor's plasticity energy and epistasis energy higher morning, the most also can eliminate use
Steel bar corrosion is brought potentially hazardous in armored concrete.
It is a further object of the present invention to provide a kind of for synthesizing without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid two
Property organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin preparation method at normal temperatures, the present invention is with 1,3-
Propyl sulfonic acid lactone (PS, C3H6O3And N, N-dimethylaminoethyl methacrylate (DMAEMA, C S)8H12NO2) single for reaction
Body, by single step reaction at 25 DEG C, is prepared for a kind of for synthesizing without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid
Both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin.Prepared both sexes organic active monomer methyl-prop
Alkene acyloxyethyl dimethyl propylene ichthyodin, on its molecular structure in addition to containing unsaturated ethylene thiazolinyl group, contains the most simultaneously
Tertiary amine base cation group and sulfonic group anionic group.
First technical scheme of the present invention is, one is used for synthesizing and subtracts without chloride ion amphoteric poly-carboxylic high-performance
The both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin of water preparation, its molecular structure is:
。
It is a further object of the present invention to provide a kind of for synthesizing without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid
Both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin preparation method at normal temperatures, concrete steps are such as
Under:
First 1,3-propyl sulfonic acid internal ester monomer (purity is more than 99%) and N, the N-dimethylamino first of different amounts are weighed
Base acrylic acid ethyl ester monomer (purity is more than 99%), is dissolved separately in the acetone reaction dissolvent of 40mL preparation 1,3-propyl group
Sultones monomer acetone soln and N, N-dimethylaminoethyl methacrylate monomer acetone soln；Use different charging side
Formula, 1 will prepared in advance, 3-propyl sulfonic acid internal ester monomer acetone soln and N, N-dimethylaminoethyl methacrylate monomer
Acetone soln joins in round-bottomed flask, sealing, at 25 DEG C, and lucifuge single step reaction certain time；Ice-water bath cooling, sucking filtration,
After being vacuum dried 24h at 25 DEG C after low temperature washing with acetone 3 times again, obtain a kind of for synthesizing without the poly-carboxylic of chloride ion amphoteric
The both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin finished product of acid high-performance water reducing agent.
Preferably, 1 in described step, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate
Monomer mole ratio is (0.75～1.25): 1.
Preferably, the different feed way in described step are with acetone reaction dissolvent for end liquid, are sequentially added into N, N-bis-
Methyaminomethyl acrylic acid ethyl ester monomer and 1,3-propyl sulfonic acid internal ester monomer；It is initially charged N, N-dimethylamino methyl acrylic acid
Acetate monomer acetone soln is slowly added dropwise 1,3-propyl sulfonic acid internal ester monomer acetone soln again；It is initially charged in 1,3-propyl sulfonic acid
Ester monomer acetone soln is slowly added dropwise N, N-dimethylaminoethyl methacrylate monomer acetone soln again.
Preferably, the lucifuge single step reaction time at 25 DEG C in described step is 36～60h.
Below in conjunction with specific embodiment, the application principle of the present invention is further described.
Embodiment 1
Accurately weigh 1,3-propyl sulfonic acid internal ester monomer (purity is more than 99%) and the N of 9.4g, N-dimethylamino methyl third
Olefin(e) acid acetate monomer (purity is more than 99%), is dissolved separately in the acetone reaction dissolvent of 40mL preparation 1,3-propyl sulfonic acid
Internal ester monomer acetone soln and N, N-dimethylaminoethyl methacrylate monomer acetone soln；Use different feed way, will
The 1,3-propyl sulfonic acid internal ester monomer acetone soln prepared in advance and N, N-dimethylaminoethyl methacrylate monomer acetone
Solution joins in round-bottomed flask, sealing, lucifuge single step reaction certain time at 25 DEG C；Ice-water bath cooling, sucking filtration, then through low
After being vacuum dried 24h at 25 DEG C after temperature washing with acetone 3 times, obtain a kind of for synthesizing without chloride ion amphoteric polycarboxylic acids height
The both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin finished product of energy water reducer.
Preferably, 1 in described step, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate
Monomer mole ratio is 1.00: 1.
Preferably, the different feed way in described step for being initially charged N, N-dimethylaminoethyl methacrylate list
Body acetone soln is slowly added dropwise 1,3-propyl sulfonic acid internal ester monomer acetone soln again.
Preferably, the lucifuge single step reaction time at 25 DEG C in described step is 48h.
Obtain is a kind of for synthesizing the both sexes organic active monomer without chloride ion amphoteric high performance water reducing agent of polyocarboxy acid
The molecular structure of methylacryoyloxyethyl dimethyl propylene ichthyodin is:
。
Embodiment 2
Substantially the same manner as Example 1, different is:
Preferably, 1 in described step, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer
Mol ratio is 0.75: 1.
Preferably, the different feed way in described step are with acetone reaction dissolvent for end liquid, are sequentially added into N, N-bis-
Methyaminomethyl acrylic acid ethyl ester monomer and 1,3-propyl sulfonic acid internal ester monomer.
Preferably, the lucifuge single step reaction time at 25 DEG C in described step is 36h.
Embodiment 3
Substantially the same manner as Example 1, except for the difference that:
Preferably, 1 in described step, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer
Mol ratio is 0.75: 1.
Embodiment 4
Substantially the same manner as Example 1, except for the difference that:
Preferably, 1 in described step, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer
Mol ratio is 0.75: 1.
Preferably, the different feed way in described step for being initially charged 1,3-propyl sulfonic acid internal ester monomer acetone soln
It is slowly added dropwise N, N-dimethylaminoethyl methacrylate monomer acetone soln again.
Preferably, the lucifuge single step reaction time at 25 DEG C in described step is 60h.
Embodiment 5
Substantially the same manner as Example 1, except for the difference that:
Preferably, the different feed way in described step are with acetone reaction dissolvent for end liquid, are sequentially added into N, N-diformazan ammonia
Amino ethyl methacrylate monomer and 1,3-propyl sulfonic acid internal ester monomer.
Preferably, the lucifuge single step reaction time at 25 DEG C in described step is 60h.
Embodiment 6
Substantially the same manner as Example 1, except for the difference that:
Preferably, the lucifuge single step reaction time at 25 DEG C in described step is 36h.
Embodiment 7
Substantially the same manner as Example 1, except for the difference that:
Preferably, the different feed way in described step are for being initially charged 1, and 3-propyl sulfonic acid internal ester monomer acetone soln delays again
Slowly N, N-dimethylaminoethyl methacrylate monomer acetone soln is dripped.
Embodiment 8
Substantially the same manner as Example 1, except for the difference that:
Preferably, 1 in described step, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer
Mol ratio is 1.25: 1.
Preferably, the different feed way in described step are with acetone reaction dissolvent for end liquid, are sequentially added into N, N-bis-
Methyaminomethyl acrylic acid ethyl ester monomer and 1,3-propyl sulfonic acid internal ester monomer.
Embodiment 9
Substantially the same manner as Example 1, except for the difference that:
Preferably, 1 in described step, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer
Mol ratio is 1.25: 1.
Preferably, the lucifuge single step reaction time at 25 DEG C in described step is 60h.
Embodiment 10
Substantially the same manner as Example 1, different is:
Preferably, 1 in described step, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer
Mol ratio is 1.25: 1.
Preferably, the different feed way in described step for being initially charged 1,3-propyl sulfonic acid internal ester monomer acetone soln
It is slowly added dropwise N, N-dimethylaminoethyl methacrylate monomer acetone soln again.
Preferably, the lucifuge single step reaction time at 25 DEG C in described step is 36h.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (5)
1. a methylacryoyloxyethyl dimethyl propylene ichthyodin, it is characterised in that this methylacryoyloxyethyl dimethyl
Propane sulfonic acid ammonium molecular structure is:
。
2. the preparation method of a methylacryoyloxyethyl dimethyl propylene ichthyodin as claimed in claim 1, it is characterised in that
The preparation method of this methylacryoyloxyethyl dimethyl propylene ichthyodin comprises the following steps:
First the 1 of different amounts is weighed, 3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer,
Being dissolved separately in compound concentration in the acetone reaction dissolvent of 40mL is 1.125～1.875mol L-11,3-propyl sulfonic acid in
Ester monomer acetone soln and N, N-dimethylaminoethyl methacrylate monomer acetone soln；
Use different feed way, 1 will prepared in advance, 3-propyl sulfonic acid internal ester monomer acetone soln and N, N-dimethylamino
Ethyl methacrylate monomer acetone soln joins in round-bottomed flask, sealing, at 25 DEG C, and lucifuge single step reaction one timing
Between；
Reaction end is placed on frozen water bath and cools down, and separates out product and is placed on pressure-reduction filter device sucking filtration, then through low temperature-10
DEG C～the washing with acetone 3 times of 10 DEG C after, then at 25 DEG C, be vacuum dried 24h, obtain a kind of for synthesizing without chloride ion amphoteric
The both sexes organic active monomer methylacryoyloxyethyl dimethyl propylene ichthyodin finished product of high performance water reducing agent of polyocarboxy acid.
3. the preparation method of methylacryoyloxyethyl dimethyl propylene ichthyodin as claimed in claim 2, it is characterised in that institute
State 1,3-propyl sulfonic acid internal ester monomer and N, N-dimethylaminoethyl methacrylate monomer mole ratio is 0.75～1.25: 1.
4. the preparation method of methylacryoyloxyethyl dimethyl propylene ichthyodin as claimed in claim 2, it is characterised in that institute
Stating different feed way is: with acetone reaction dissolvent for end liquid, be sequentially added into N, N-dimethylaminoethyl methacrylate monomer
With 1,3-propyl sulfonic acid internal ester monomer；It is initially charged N, N-dimethylaminoethyl methacrylate monomer acetone soln the most slowly to drip
Add 1,3-propyl sulfonic acid internal ester monomer acetone soln；Or be initially charged 1,3-propyl sulfonic acid internal ester monomer acetone soln and the most slowly drip
Add N, N-dimethylaminoethyl methacrylate monomer acetone soln.
5. the preparation method of methylacryoyloxyethyl dimethyl propylene ichthyodin as claimed in claim 2, it is characterised in that institute
The lucifuge single step reaction time at 25 DEG C of stating is 36 h～60h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109627395A (en) * | 2018-12-14 | 2019-04-16 | 中科院广州化学有限公司南雄材料生产基地 | A kind of both sexes polycarboxylate water-reducer and preparation method |
| CN110818835A (en) * | 2019-11-22 | 2020-02-21 | 中建商品混凝土有限公司 | Anti-settling auxiliary agent and preparation method and application thereof |
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