CN105669926A - Preparation method of high-content naphthalene water reducer - Google Patents

Preparation method of high-content naphthalene water reducer Download PDF

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CN105669926A
CN105669926A CN201610042466.7A CN201610042466A CN105669926A CN 105669926 A CN105669926 A CN 105669926A CN 201610042466 A CN201610042466 A CN 201610042466A CN 105669926 A CN105669926 A CN 105669926A
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naphthalene
water
reaction
concentration
water reducer
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CN105669926B (en
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季根忠
章思怡
戚天木
来超超
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University of Shaoxing
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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
    • C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
    • C08G16/02—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
    • C08G16/0212—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds
    • C08G16/0218—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds containing atoms other than carbon and hydrogen
    • C08G16/0237—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes with acyclic or carbocyclic organic compounds containing atoms other than carbon and hydrogen containing sulfur
    • 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
    • C04B24/16—Sulfur-containing compounds
    • C04B24/20—Sulfonated aromatic compounds
    • C04B24/22—Condensation or polymerisation products thereof
    • C04B24/226—Sulfonated naphtalene-formaldehyde condensation products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302—Water reducers

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a preparation method of a high-content naphthalene water reducer, comprising the following steps: sulfonation, hydrolysis, condensation, and drying after neutralization, wherein sulfonation includes: in a reactor with rectification, rectifying and sulfonating sulfuric acid 50-93% in concentration by weight with naphthalene and producing water during the sulfonation of the sulfuric acid with the naphthalene, the concentration of the sulfuric is reduced, the water is produced by rectification, the concentration of the sulfuric acid in the reactor is increased, the naphthalene is rectified back to the reactor for continual sulfonation, the whole process is balanced owing to the water production by rectification and the water production by sulfonation, and the temperature in the reactor stabilizes between 160 DEG C and 175 DEG C until the sulfuric acid in the reactor is fully consumed in reaction; the preparation method of the invention is simple and stable and has easily controllable parameters, and the produced naphthalene water reducer has stable performance and good quality.

Description

A kind of preparation method of high-load naphthalene water reducer
Technical field:
The invention belongs to building material field, the preparation method relating to a kind of chemical admixture, the preparation method being specifically related to a kind of high-load naphthalene water reducer.
Background technology:
Cement water reducing agent is under concrete workability and cement consumption permanence condition, can reduce mixing water amount, improve concrete strength, save the additive of cement consumption. Naphthalene water reducer is to make consumption a kind of high efficiency water reducing agent maximum, most widely used on domestic market. According to statistics, the secondary water reducers such as naphthalene systems in 2009 account for all synthesis water reducer total outputs 67.5%, within 2010, it is 67.1%, within 2011, it is 66.5%, although proportion declines year by year, but its price is relatively cheap, and good with early strength agent, retarder compound property, multi-functional composite superplasticizer can be formed, commercially still extensive at present.
The preparation method of current naphthalene water reducer obtains product through dry after mainly including the reactions such as sulfonation, hydrolysis, condensation, neutralization. It is low that the method obtains naphthalene water reducer concentration, about contains the sodium sulfate (accounting for powder) of quality 20～25%, makes concrete slump loss strengthen, and is unsuitable for gravitational grouting and preparation pump concrete, affects construction speed and quality. Na in the naphthalene water reducer product that concentration is low2SO4Crystallization can be produced below 15 DEG C, have a strong impact on concrete metering pump precision and water-reducing effect. In order to reduce crystallization degree in product and reduce crystalline polamer, many production technologies increase the operation of low temperature sucking filtration by Na2SO4Remove.
The high-quality naphthalene water reducer low for manufacturing sulphates content, industrial commonly used calcium desulfurization method carrys out removing sulfate. Na is reduced as patent CN103755203A provides in a kind of naphthalene water reducer preparation process2SO4Way: synthesize low dense naphthalene water reducers by sulfonation, hydrolysis, condensation, four operations of neutralization, then through calcium sulfate precipitation separation process, prepare highly concentrated naphthalene water reducer. But producing another one problem is exactly: consequent calcium sulfate waste residues, serious pollution of ecological environment, too increases equipment and production cost simultaneously.
CN104497250A proposes the consumption adopting binary azeotropic method to reduce concentrated sulphuric acid, makes sulfuric acid sulfonation reaction thoroughly, thus reducing Na in product2SO4The content of content.But in fact a lot of data show that naphthalene and water do not have azeotropism, experiment to also indicate that naphthalene and water can not form azeotropic, prepare distillation water-scavenging capability in water reducer process limited. Additionally under the high temperature of 140～160 DEG C, easily there is the side reactions such as oxidation reaction, and the LOMAR PWA EINECS 246-676-2 generation secondary sulfonation being previously generated in concentrated sulphuric acid and naphthalene, makes the utilization rate of naphthalene decline; Due to the dehydration of concentrated sulphuric acid, under high temperature, the LOMAR PWA EINECS 246-676-2 generated in advance is also easily reacted the side reactions such as generation sulfone further occur with naphthalene, makes the performance of water reducer reduce.
Adopt ethanol to make accelerator from naphthalene water reducer, isolate Na2SO4, it is suitable for when higher temperature (75 DEG C) and water reducer total concentration high as far as possible and carries out, add short analysis agent by the 20% of water preparation quality, Na can be made2SO4Content is down to less than 3%.
Summary of the invention:
Produce that waste material is difficult for above-mentioned traditional high concentration and high efficiency naphthalene water reducer, the defect such as oxidation, secondary sulfonation in technical process, the present invention provides a kind of method with low-concentration sulfuric acid for raw material production high concentration and high efficiency naphthalene water reducer.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
The preparation method of a kind of high-load naphthalene water reducer, it is characterised in that comprise the following steps:
(1) sulfonation:
In the reactor with rectification, by the rectification carry out sulfonating reaction together with naphthalene of sulphuric acid that mass percent concentration is 50～93%, sulphuric acid and naphthalene carry out sulfonating reaction, are simultaneously generated water, and sulfuric acid concentration declines, by rectification recovered water, improving the sulfuric acid concentration in still, naphthalene returns to evaporate and proceeds sulfonating reaction into reactor, owing to rectification recovered water, sulfonation generate water and reach balance in whole process, temperature in the kettle is stable between 160～175 DEG C, until sulfuric acid reaction consumption is complete in still;
(2) hydrolysis:
After sulfonating reaction, the α LOMAR PWA EINECS 246-676-2 of residual adds water generation hydrolysis, and hydrolysis time is 0～0.5h, and temperature is 100～140 DEG C;
(3) condensation: in the hydrolysis product obtain step (2), adds paraformaldehyde and water generation condensation reaction;
(4) neutralize: step (3) condensation reaction products is regulated pH value to 6-8, dry, obtain high-load naphthalene water reducer.
Further it is provided that
In step (1): the mol ratio of naphthalene and sulphuric acid is 1:0.95～1.15; Sulfonating reaction temperature is preferably 160～165 DEG C, and the time is 2～10.0h.
In step (1): sulfonating reaction and rectifying and dewatering process carry out simultaneously, ensure the concentration of sulfonating agent sulphuric acid.
Under 1atm, the sulphuric acid boiling point of mass concentration 60% is 142 DEG C, and the sulphuric acid boiling point of mass concentration 70% is 170 DEG C, when temperature in the kettle is 160～165 DEG C, the concentration of sulphuric acid is 65～68%, and it is corresponding sulfonic acid that the sulphuric acid of this concentration can be used as sulfonating agent by naphthalene sulfonation.
Due to the fact that employing sulfonating reaction carries out with rectifying and dewatering process simultaneously, therefore without selecting concentrated sulphuric acid, when sulfuric acid concentration does not reach sulfonating reaction desired concn, pass through rectifying and dewatering, water is light component, in distillation process, from rectifying tower top extraction, sulfuric acid concentration in still rises, and temperature in the kettle rises; When temperature in the kettle rises most 160～175 DEG C, sulphuric acid and naphthalene generation sulfonating reaction, it is simultaneously generated water, now, sulfuric acid concentration declines, so, owing to rectification recovered water, sulfonation generate water and reach balance in whole process, temperature in the kettle is stable between 160～175 DEG C, until sulfuric acid reaction consumption is complete in still.
In step (1): in distillation process, a recovered water in rectifying tower top distillate, upper strata naphtalene oil returns to evaporate and carries out sulfonating reaction into reactor.
Owing to naphthalene all has higher vapour pressure in various temperature, in rectification removal process, the also vaporization simultaneously of part naphthalene enters tower top. The fusing point of naphthalene is up to 80 DEG C, and rectifying tower top mixed vapour out need to cool down with the hot water of 80～95 DEG C, and is incubated distillate at 80～85 DEG C, it is prevented that the phenomenons such as gambling plug occur. Additionally naphthalene needs after being condensed together with water, with a gun barrel, to be gone out by the hydromining of tank middle and lower part, and the naphthalene of tank middle and upper part returns sulfonating reaction still, carries out further sulfonating reaction.
In described step (2): the time of hydrolysis is very short is 0～0.5h, and temperature is 100～140 DEG C, the step that namely can not be hydrolyzed (when hydrolysis time is 0), and it is made directly the condensation of step (3).
Owing to sulfonating reaction is a reversible reaction, the poor stability of α LOMAR PWA EINECS 246-676-2, hydrolysis rate is more than β LOMAR PWA EINECS 246-676-2. Low-concentration sulfuric acid is in rectification concentration process, and α LOMAR PWA EINECS 246-676-2 is also hydrolyzed simultaneously, and after therefore sulfonation terminates, α LOMAR PWA EINECS 246-676-2 content is low, and β LOMAR PWA EINECS 246-676-2 content is high. Therefore produce different from traditional water reducer, it is possible to be not hydrolyzed reaction, or hydrolysis time is very short, it is possible to completes within the 0.5h time.
The operation principle of the present invention and having the beneficial effect that:
1, the present invention adopts low-concentration sulfuric acid to be raw material, dilute sulfuric acid rectification concentration is utilized and sulfonating reaction combines, produce high concentration and high efficiency naphthalene water reducer;
The present invention is by dilute sulfuric acid rectification together with naphthalene, and in distillation process, water is light component, and from rectifying tower top extraction, the sulfuric acid concentration in still rises, and rectifying still temperature rises. H 2 so 4 concentration when in still > 63% time, the temperature in still is about 150～175 DEG C. At this temperature, sulphuric acid and naphthalene generation sulfonating reaction, it is simultaneously generated water, makes sulfuric acid concentration decline. Whole process is rectification recovered water, and sulfonation generates water and reaches balance, makes the temperature stabilization in still without further up between 150～175 DEG C. Along with in still, sulfuric acid reaction runs out of, sulfonating reaction is no longer occurred to generate water, system temperature just can be further up, thus the sulphuric acid concentration avoided needs high temperataure phenomena (> 180 DEG C), make dilute sulfuric acid concentration be gradually increasing additionally, due to rectifying and dewatering effect and ensure sulfonation ability, make naphthalene sulfonating reaction thorough; Therefore can quantitative response between naphthalene and sulphuric acid, it is not necessary to add excessive sulphuric acid, it is achieved energy-saving and cost-reducing.
2, the low-concentration sulfuric acid (concentration is 50～93%) adopting non-oxidation ability, sulfonation ability relatively weak is sulfonating agent; The sulphuric acid of low concentration it also avoid LOMAR PWA EINECS 246-676-2 and reacts the possibility generating sulfone further with naphthalene.
3, the naphthalene of the present invention controls in 1:(0.95～1.15 with the ratio of sulfonating agent sulphuric acid), 1:(1.3～1.4 that ratio is more traditional) have and significantly decline, so that the content of sodium sulfate is reduced to less than 10% in product, it is possible to product quality is greatly improved, adapt to the requirement of winter construction.
4, the hydrolysis time of step of the present invention (2) is short, it might even be possible to need not be hydrolyzed step, and is made directly the condensation of step (3), which saves operation and time.
It is described further below in conjunction with detailed description of the invention.
Detailed description of the invention:
Embodiment 1:
134g crude naphthalene (purity >=95% is added in reaction bulb, 1.0mol), 114g sulphuric acid (mass concentration: 90%, 1.05mol), with the rectifying column of 20cm on reaction bulb, it is warmed up to 160～170 DEG C of reactive distillation 3h, period recovered water 16g, reaction adds a certain amount of water after terminating, and is hydrolyzed 0.5h at 110 DEG C, and after hydrolysis, Controlled acidity is 28%.After cooling to 90 DEG C, add 34.4g paraformaldehyde (purity >=96%, 1.1mol is in formaldehyde) and 58.5g water, be warmed up to 100～105 DEG C gradually, be incubated 4h, insulating process add water management and is polymerized under suitable viscosity. Reaction adds liquid caustic soda and regulates pH=6～8 after terminating, dry, obtains naphthalene water reducer.
Embodiment 2:
134g crude naphthalene (purity >=95%, 1.0mol), 178.0g sulphuric acid (mass concentration: 55% is added in reaction bulb, 1.0mol), it is warmed up to 135 DEG C and starts back to evaporate, recovered water, continuing rectification and be warmed up to 165～175 DEG C of reaction 9h, after reaction terminates, recording acidity is 26%. Cool to 95 DEG C, add 30.7g paraformaldehyde (purity >=99%, 1mol is in formaldehyde) and 54.0g water, be warmed up to 100～110 DEG C gradually, be incubated 8h, insulating process add water management and is polymerized under suitable viscosity. Reaction adds liquid caustic soda and regulates pH=6～8 after terminating, dry, obtains naphthalene water reducer.
Embodiment 3:
134.7g crude naphthalene (purity >=95%, 1.0mol), 147.0g concentrated sulphuric acid (mass concentration: 70% is added in reaction bulb, 1.05mol), being warmed up to 170～175 DEG C of reaction 1.5h, reaction adds a certain amount of water after terminating, being hydrolyzed 0.5h at 120 DEG C, after hydrolysis, Controlled acidity is 26%. After cooling to 90 DEG C, add 40.6g paraformaldehyde (purity >=96%, 1.3mol is in formaldehyde) and 40.6g water, be warmed up to 115～120 DEG C gradually, be incubated 8h, insulating process add water management and is polymerized under suitable viscosity. Reaction adds liquid caustic soda and regulates pH=6～8 after terminating, dry, obtains naphthalene water reducer.
Comparative example 1: adopt the technology of CN103755203A to prepare high-concentration naphthalene based water reducer.
It is chloroazotic acid 10-25 part in parts by weight, crude naphthalene 35-50 part, formaldehyde 12-16 part, the proportioning of sodium hydroxide 3-5 part takes each raw material, low dense naphthalene water reducer is synthesized by sulfonation, hydrolysis, condensation, four operations of neutralization, then through calcium sulfate precipitation separation process, prepare highly concentrated naphthalene water reducer. Obtain calcium sulfate solid waste 6-8 part, it is necessary to landfill disposal simultaneously.
Comparative example 2: adopt the technology of CN104497250A to prepare high-concentration naphthalene based water reducer.
1, according to parts by weight meter, in reactor, 160 parts of liquid industrial naphthalenes are added, when stirring and be warming up to 135 DEG C, starting to drip 120 parts of concentration is the sulphuric acid of 98%, controls to add speed, makes temperature less than 165 DEG C, insulation binary azeotropic backflow 4h, Controlled acidity is 25%; " azeotropic " obtains 18 parts of needs extra process of waste water (dilute sulfuric acid solution) simultaneously.
2, step 1 gained material being cooled to 115 DEG C, then add 23 parts of water in reactor, be to slowly warm up to 130 DEG C, utilize binary azeotropic method to reclaim naphthalene, Controlled acidity is 26% stopping hydrolysis;
3, step 2 gained material being cooled to 110 DEG C, start to drip 100 parts of formaldehyde, control rate of addition, dropwise in 3 hours, then insulation condensation 5 hours, reclaims formaldehyde simultaneously in this step process;
4, add 170 parts of alkali to step 3 gained condensation substance to neutralize, be then drying to obtain finished product.
Application and performance detection:
The naphthalene water reducer prepared by embodiment of the present invention 1-3, prepares high-concentration naphthalene based water reducer with prior art, carries out performance Indexs measure and statistics respectively, as shown in table 1:
Cement: P II 52.5, Zhejiang spike Cement Co., Ltd, fine aggregate: sand, particle diameter 0～5mm. Coarse aggregate: limestone gravel, particle diameter 5～10mm.Test is undertaken by the regulation of GB8077-2000 " Methods for testing uniformity of concrete admixture ", and wherein sodium sulfate is by the gravimetric detemination in standard.
Table 1: the embodiment of the present invention compares with the performance of prior art
Sequence number Na2SO4Content m% Fluidity/mm(0.5h) Remarks
Embodiment 1 8.7 216 Solid waste without calcium sulfate, without acid-bearing wastewater
Embodiment 2 6.8 222 Solid waste without calcium sulfate, without acid-bearing wastewater
Embodiment 3 8.1 210 Solid waste without calcium sulfate, without acid-bearing wastewater
Comparative example 1 7.5 212 Increase processing step, increase calcium sulfate solid waste
Comparative example 2 21.6 178 Increasing acid-bearing wastewater, side reaction generates sulfone
As shown in table 1: naphthalene water reducer prepared by the present invention, compared with high-concentration naphthalene based water reducer prepared by prior art:
1, sulfuric acid dosage is few, and the sulfuric acid concentration of use is low.
The low-concentration sulfuric acid (concentration is 50～93%) that the present invention adopts non-oxidation ability, sulfonation ability relatively weak is sulfonating agent; The sulphuric acid of low concentration it also avoid LOMAR PWA EINECS 246-676-2 and reacts the possibility generating sulfone further with naphthalene.
2, sodium sulphate content is low, and fluidity is high.
The ratio of the naphthalene of the present invention and sulfonating agent sulphuric acid controls in 1:(0.95～1.15), 1:(1.3～1.4 that ratio is more traditional) have and significantly decline, so that the content of sodium sulfate is reduced to less than 10% in product, fluidity is higher, product quality can be greatly improved, adapt to the requirement of winter construction.
3, produce without solid waste or acid-bearing wastewater.
Instant invention overcomes traditional handicraft and be easily generated the technological deficiency of calcium sulfate solid waste and acid-bearing wastewater, there is better environmental-protecting performance.

Claims (6)

1. the preparation method of a high-load naphthalene water reducer, it is characterised in that comprise the following steps:
(1) sulfonation:
In the reactor with rectification, by the rectification carry out sulfonating reaction together with naphthalene of sulphuric acid that mass percent concentration is 50～93%, sulphuric acid and naphthalene carry out sulfonating reaction, are simultaneously generated water, and sulfuric acid concentration declines, by rectification recovered water, improving the sulfuric acid concentration in still, naphthalene returns to evaporate and proceeds sulfonating reaction into reactor, owing to rectification recovered water, sulfonation generate water and reach balance in whole process, temperature in the kettle is stable between 160～175 DEG C, until sulfuric acid reaction consumption is complete in still;
(2) hydrolysis:
After sulfonating reaction, the α LOMAR PWA EINECS 246-676-2 of residual adds water generation hydrolysis, and hydrolysis time is 0～0.5h, and temperature is 100～140 DEG C;
(3) condensation: in the hydrolysis product obtain step (2), adds paraformaldehyde and water generation condensation reaction;
(4) neutralize: step (3) condensation reaction products is regulated pH value to 6-8, dry, obtain high-load naphthalene water reducer.
2. the preparation method of a kind of high-load naphthalene water reducer according to claim 1, it is characterised in that: in step (1): the mol ratio of naphthalene and sulphuric acid is 1:0.95～1.15; Sulfonating reaction temperature is 160～165 DEG C, and the time is 2～10.0h.
3. the preparation method of a kind of high-load naphthalene water reducer according to claim 1, it is characterised in that: in step (1): sulfonating reaction and rectifying and dewatering process carry out simultaneously, ensure the concentration of sulfonating agent sulphuric acid.
4. the preparation method of a kind of high-load naphthalene water reducer according to claim 1, it is characterised in that: in step (1): in distillation process, a recovered water in rectifying tower top distillate, upper strata naphtalene oil returns to evaporate and carries out sulfonating reaction into reactor.
5. the preparation method of a kind of high-load naphthalene water reducer according to claim 4, it is characterized in that: rectifying tower top mixed vapour out cools down with the hot water of 80～95 DEG C, and distillate is incubated at 80～85 DEG C, prevent the phenomenons such as gambling plug from occurring, naphthalene be condensed together with water after with a gun barrel, the hydromining of tank middle and lower part is gone out, and the naphthalene of tank middle and upper part is returned sulfonating reaction still, carry out further sulfonating reaction.
6. the preparation method of a kind of high-load naphthalene water reducer according to claim 1, it is characterised in that: in described step (2): the time of hydrolysis is 0, be not namely hydrolyzed step, and is made directly the condensation of step (3).
CN201610042466.7A 2016-01-22 2016-01-22 A kind of preparation method of high-content naphthalene water reducer Active CN105669926B (en)

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CN106432661A (en) * 2016-09-18 2017-02-22 江苏苏博特新材料股份有限公司 Modified naphthalene water reducer and preparation method thereof
CN106746861A (en) * 2016-12-23 2017-05-31 河南奥思达新材料有限公司 A kind of naphthalene water reducer and its preparation technology
CN107573471A (en) * 2017-08-31 2018-01-12 浙江吉盛化学建材有限公司 A kind of production technology of FDN high efficiency water reducing agents
CN108530271A (en) * 2018-05-31 2018-09-14 山西豪仑科化工有限公司 A kind of naphthalene method of sulfonating of coproduction 1- naphthols and beta naphthal

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CN101898926A (en) * 2009-05-25 2010-12-01 浙江五龙化工股份有限公司 Sulfonation process for producing dye dispersant and concrete water reducing agent
CN102351458A (en) * 2011-07-14 2012-02-15 兰州大学 Method for preparing water reducer by using low distillate section of neutral wash oil instead of industrial naphthalene
CN104557537A (en) * 2014-12-04 2015-04-29 江门谦信化工发展有限公司 Method for producing butyl acrylate by reaction and rectification in tower

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Publication number Priority date Publication date Assignee Title
CN101898926A (en) * 2009-05-25 2010-12-01 浙江五龙化工股份有限公司 Sulfonation process for producing dye dispersant and concrete water reducing agent
CN102351458A (en) * 2011-07-14 2012-02-15 兰州大学 Method for preparing water reducer by using low distillate section of neutral wash oil instead of industrial naphthalene
CN104557537A (en) * 2014-12-04 2015-04-29 江门谦信化工发展有限公司 Method for producing butyl acrylate by reaction and rectification in tower

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106432661A (en) * 2016-09-18 2017-02-22 江苏苏博特新材料股份有限公司 Modified naphthalene water reducer and preparation method thereof
CN106432661B (en) * 2016-09-18 2019-04-02 江苏苏博特新材料股份有限公司 A kind of modified naphthalene series water-reducing agent and preparation method thereof
CN106746861A (en) * 2016-12-23 2017-05-31 河南奥思达新材料有限公司 A kind of naphthalene water reducer and its preparation technology
CN106746861B (en) * 2016-12-23 2020-01-31 平顶山奥思达科技有限公司 naphthalene series water reducing agent and preparation process thereof
CN107573471A (en) * 2017-08-31 2018-01-12 浙江吉盛化学建材有限公司 A kind of production technology of FDN high efficiency water reducing agents
CN107573471B (en) * 2017-08-31 2019-10-29 浙江吉盛化学建材有限公司 A kind of production technology of FDN high efficiency water reducing agent
CN108530271A (en) * 2018-05-31 2018-09-14 山西豪仑科化工有限公司 A kind of naphthalene method of sulfonating of coproduction 1- naphthols and beta naphthal

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