CN103910831B - Method for producing polycarboxylate water reducer from oxalic acid - Google Patents
Method for producing polycarboxylate water reducer from oxalic acid Download PDFInfo
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- CN103910831B CN103910831B CN201410013561.5A CN201410013561A CN103910831B CN 103910831 B CN103910831 B CN 103910831B CN 201410013561 A CN201410013561 A CN 201410013561A CN 103910831 B CN103910831 B CN 103910831B
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- oxalic acid
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- deionized water
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 title claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 235000006408 oxalic acid Nutrition 0.000 title claims abstract description 15
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 title abstract description 23
- 238000004519 manufacturing process Methods 0.000 title abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract 2
- 239000003643 water by type Substances 0.000 claims description 8
- 208000014903 transposition of the great arteries Diseases 0.000 claims description 7
- 238000002411 thermogravimetry Methods 0.000 claims description 5
- 238000012032 thrombin generation assay Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 abstract description 15
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 abstract 2
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000004567 concrete Substances 0.000 description 8
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 6
- 239000004568 cement Substances 0.000 description 6
- 239000004566 building material Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000003467 diminishing effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- SUBDBMMJDZJVOS-UHFFFAOYSA-N 5-methoxy-2-{[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]sulfinyl}-1H-benzimidazole Chemical compound N=1C2=CC(OC)=CC=C2NC=1S(=O)CC1=NC=C(C)C(OC)=C1C SUBDBMMJDZJVOS-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 241000555268 Dendroides Species 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920005551 calcium lignosulfonate Polymers 0.000 description 1
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011376 self-consolidating concrete Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a method for producing a polycarboxylate water reducer from oxalic acid. The method comprises the following steps of 1, adding TPEG and deionized water into a reactor according to a ratio of 1: 2, heating the materials in the reactor to a temperature of 60 DEG C, and stirring the materials until complete dissolution for next use, 2, preparing a material A by fully mixing 23-27kg of deionized water, 0.7-1.2kg of mercaptoacetic acid and 0.4-0.8kg of oxalic acid and preparing a material B by fully mixing 18-22kg of deionized water and 33-36kg of acrylic acid, and 3, respectively and slowly adding the material A and the material B into the reactor used in the step 1 in 2.8-3.2h in a way that 50wt% of the material A is firstly added into the reactor and is subjected to temperature keeping at a temperature of 58-62 DEG C for 0.7-1.0h and then the rest of the material A is added into the reactor, carrying out a polymerization reaction process for 0.8-1.0h, adding sodium hydroxide into the reaction product, carrying out a reaction process for 0.9-1.0h, adjusting a pH value to 8-10 and carrying out discharging to obtain a finished product.
Description
Technical field
The present invention relates to polycarboxylate dehydragent, especially with the preparation of oxalic acid, the method stable operation makes product exist
The superiority of quality is highlighted in the use of concrete admixture.
Background technology
Water reducer is a kind of important concrete admixture, is one of staple product of building material pillar industry.Poly- carboxylic
Sour series high-performance dehydragent is developed after high efficiency water reducing agent after the ordinary water-reducing agent that calcium lignosulfonate is representative and with naphthalene system as representative
The third generation high-performance water reducing agent for getting up, a kind of efficient diminishing that scientific and technological content highest, application prospect are best, combination property is optimal
Agent, as the representative kind of the water reducer of new generation developed in worldwide, the polycarboxylate water-reducer of Japan is
Instead of the status of naphthalene water reducer.
The widely used high efficiency water reducing agent of current China is mainly naphthalene system product, and naphthalene series high-efficiency water-reducing agent is to improving building
Quality and service life, reducing energy consumption, save cement and reduce the aspect such as environmental pollution and all play an important role, but naphthalene
Based water reducer also exposes some problems for itself being difficult to overcome in the development of recent decades, for example, being collapsed with the concrete that it is prepared
Degree of falling loss influence is fairly obvious, it is impossible to have water-reducing rate higher, and the primary raw material-naphthalene of its production is the pair of coking industry
Product, source is restricted by steel and iron industry, and China is formulating the standard of polycarboxylate high performance water-reducing agent, with the poly- carboxylic of specification
The manufacturing quick, sound development of sour based water reducer.
Literature search is disclosed：①《The development of polycarboxylate high-efficiency water reducing agent（Ⅱ）The synthesis of-copolymer and sign》Author：
Kingdom builds Wei Jingliang《Journal of Building Materials》2006 the 4th phases；②《Esterification process prepares grinding for polycarboxylate high-efficiency water-reducing agent afterwards
Study carefully》, author：It is white that kingdom builds Ma Zhiping envelopes《New Building Materials》2006 the 4th phases, the technology is the work to energy generation environment destruction
The recycling of industry waste material, and the use of high energy consumption material in production is reduced, and the solid that will can be produced in process of production
Slag makes full use of and is made early strength agent, is a kind of brand-new, environmental protection, energy-conservation high efficiency water reducing agent production method.
Polycarboxylate high performance water-reducing agent of the invention is carboxylic acids graft polyol copolymer and other effective auxiliary agents are answered
With product, with intensity is high, heat resistance, durability and the features such as good slump retaining, can well solve diminishing, bleed, slow setting, secrete
The problems such as water, more slags or flyash substitution cement are can use in use, so that cost reduction；The product is to steel
Muscle non-corroding is acted on, and can significantly increase the slump of concrete, improves concrete workability, largely improves coagulation
Soil mechanics performance and the endurance quality such as impervious, for building material market provides new cheap products.
The content of the invention
It is an object of the invention to：The high performance water reducing agent of polyocarboxy acid of offer, water-reducing rate is high, it is possible to decrease concrete water
Amount, saves cement, to reinforcing bar non-hazardous, concrete shrinkage is had no adverse effects.
The object of the present invention is achieved like this：One kind produces polycarboxylate dehydragent and preparation method thereof using oxalic acid,
Implement step by step；
Step 1 adds 1 to reactor:The TPEG and deionized water of 2 ratios, are warming up to 60 DEG C, and stirring material is completely dissolved
It is standby；
Step 2 prepares A material and B material respectively：
A expects:By 23-27kg deionized waters, 0.7-1.2kg TGAs, 0.4-0.8kg oxalic acid, it is well mixed and is obtained;
B expects：By 18-22kg deionized waters, 33-36kg acrylic acid, it is well mixed and is obtained;
Be respectively added slowly in the reactor of step 1 for A material and B material by step 3, and used time 2.8-3.2h, wherein A expect at twice
Add, first add 50% accounted for from weight, at 58-62 DEG C, after constant temperature 0.7-1.0h, then add A material and account for from weight
50%, polymerisation 0.8-1.0h, continuously add sodium hydroxid reaction 0.9-1.0h, during pH to 8-10, that is, discharge, and obtain finished product.
Methods described, the ratio of mud of use is that the slump of product increases 1.0-7.5 times, saves cement 1.0-1.5%.
Methods described is obtained the national standard that product has reached GB8076-2008.
Methods described select TGA, oxalic acid, be all goodization chemical plant production；TPEG is Liaoning Losec for polymeric monomer
Chemical plant produces.
Know-why of the invention and effect：Polycarboxylic acids（Salt）The molecule of water reducer is artificially formed by " MOLECULE DESIGN "
" pectination " or " dendroid " structure, and many side chains for having certain length and rigidity are connected on molecular backbone（Side chain）,
Also there are the sulfonate or other groups that cement granules can be made powered on main chain, conventional water reducing agents can be played a part of, it is heavier
What is wanted is adsorbed after cement particle surface once main chain, and side chain forms crossings on different level with the side chain of other particle surfaces, hinders
Particle is close to each other, so as to reaching dispersion（That is diminishing）Effect, this steric hindrance effect is not weakened with time lengthening, because
This, the peptizaiton of polycarboxylate water-reducer is more lasting, and the service behaviour of concrete shows more excellent than naphthalene water reducer, stream
More preferably, especially when self-compacting concrete is prepared, advantage becomes apparent dynamic and pump-conveying property, shows technological progress.
Specific embodiment
With reference to embodiment, the invention is further described.
Embodiment 1
1）1 is added to reactor:The TPEG and deionized water of 2 ratios, are warming up to 60 DEG C, and stirring treats that material all dissolves,
It is standby；
2）Then distinguish dispensing A with two gravity tanks to expect and B material：
25kg deionized waters are taken, added 0.9kg TGAs, added 0.6kg oxalic acid again, be well mixed prepared A material；20kg is taken to go
Ionized water, plus 35.5kg acrylic acid, are well mixed prepared B material；
3）A material and B material are respectively added slowly to step 1）Reactor in, used time 2.8h, wherein A material are added points for 2 times, the
Add 50% 1 time, the constant temperature stirring 1.0h at 60 DEG C is added dropwise 2 times the 50% of A material, and polymerisation 0.9h terminates, and is eventually adding hydrogen-oxygen
It is 8 that neutralization reaction 1h, pH are received in change, is got product.
Embodiment 2
1) 1 is added to reactor:The TPEG and deionized water of 2 ratios, are warming up to 60 DEG C, treat that material all dissolves, standby；
2) and then with two gravity tanks distinguish dispensing, be divided into A material and B material：
23kg deionized waters, 0.7kg TGAs, 0.4kg oxalic acid are taken, A material are well mixed to obtain;
18kg deionized waters, 33kg acrylic acid are taken, prepared B material are well mixed;
3）A material and B material are respectively added slowly to step 1）Reactor in, used time 3.0h, wherein A material are added points for 2 times, the
50% for adding from weight for 1 time, at 58 DEG C, after constant temperature 0.7h, adds for the 2nd time and to expect from the A of weight 50%, polymerisation 0.8h,
Sodium hydroxid is added, 0.9h is reacted, pH is adjusted to 9, that is, discharge to obtain finished product.
Embodiment 3
1) 1 is added to reactor:The TPEG and deionized water of 2 ratios, are warming up to 60 DEG C, treat that material all dissolves, standby；
2) and then with two gravity tanks distinguish dispensing, be divided into A material and B material：
27kg deionized waters, 1.2kg TGAs, 0.8kg oxalic acid are taken, prepared A material are well mixed;Take 22kg deionizations
Water, 36kg acrylic acid, are well mixed prepared B material;
3）A material and B material are respectively added slowly to step 1）Reactor in, used time 3.2h, wherein A material are added points for 2 times, the
50% for adding from weight for 1 time, at 62 DEG C, after constant temperature 1.0h, adds for the 2nd time and to expect from the A of weight 50%, polymerisation 1.0h,
Sodium hydroxid is added, 1.0h is reacted, pH is adjusted to 10, that is, discharge to obtain finished product.
The present invention utilizes oxalic acid（TPEG）The performance verification of the polycarboxylate dehydragent of production：The ratio of mud of use, can be bright
Aobvious increase slump, slump increases to 1.0-7.5 times, in the case of slump and the basic identical of intensity, saves water
Mud 1.0-1.5%.
This method is obtained the national standard that product has reached GB8076-2008.
This method select TGA, oxalic acid, be all goodization chemical plant production；TPEG is Liaoning Losec for polymeric monomer
Plant produced.
Claims (1)
1. a kind of method that utilization oxalic acid produces polycarboxylate dehydragent, it is characterised in that：Implement step by step；
Step 1 adds 1 to reactor:The TPEG and deionized water of 2 ratios, are warming up to 60 DEG C, and stirring material is completely dissolved standby；
Step 2 prepares A material and B material respectively：
A expects:By 23-27kg deionized waters, 0.7-1.2kg TGAs, 0.4-0.8kg oxalic acid, it is well mixed and is obtained;
B expects：By 18-22kg deionized waters, 33-36kg acrylic acid, it is well mixed and is obtained;
Be respectively added slowly in the reactor of step 1 for A material and B material by step 3, and used time 2.8-3.2h, wherein A material are thrown at twice
Plus, 50% accounted for from weight is first added, at 58-62 DEG C, after constant temperature 0.7-1.0h, then add the A material accounted for from weight 50%, polymerization
Reaction 0.8-1.0h, adds NaOH, reacts 0.9-1.0h, and pH is adjusted to 8-10, that is, discharge to obtain finished product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410013561.5A CN103910831B (en) | 2014-01-10 | 2014-01-10 | Method for producing polycarboxylate water reducer from oxalic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410013561.5A CN103910831B (en) | 2014-01-10 | 2014-01-10 | Method for producing polycarboxylate water reducer from oxalic acid |
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| CN103910831A CN103910831A (en) | 2014-07-09 |
| CN103910831B true CN103910831B (en) | 2017-05-24 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775107A (en) * | 2010-02-03 | 2010-07-14 | 北京冶建特种材料有限公司 | Preparation method of concrete polycarboxylate water-reducer at normal temperature |
| CN101974135A (en) * | 2010-10-15 | 2011-02-16 | 北京工业大学 | Normal-temperature synthesis method for polycarboxylic acid water-reducing agent |
| CN101993210A (en) * | 2010-03-04 | 2011-03-30 | 山西大学 | Prenyl polyether polycarboxylate water reducing agent and synthesis method thereof |
| CN102358763A (en) * | 2011-07-21 | 2012-02-22 | 北京工业大学 | Method for preparing additive for inhibiting side effect of clay |
-
2014
- 2014-01-10 CN CN201410013561.5A patent/CN103910831B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101775107A (en) * | 2010-02-03 | 2010-07-14 | 北京冶建特种材料有限公司 | Preparation method of concrete polycarboxylate water-reducer at normal temperature |
| CN101993210A (en) * | 2010-03-04 | 2011-03-30 | 山西大学 | Prenyl polyether polycarboxylate water reducing agent and synthesis method thereof |
| CN101974135A (en) * | 2010-10-15 | 2011-02-16 | 北京工业大学 | Normal-temperature synthesis method for polycarboxylic acid water-reducing agent |
| CN102358763A (en) * | 2011-07-21 | 2012-02-22 | 北京工业大学 | Method for preparing additive for inhibiting side effect of clay |
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