CN100430331C - Continuous production process of efficient aliphatic concrete water reducing agent - Google Patents

Continuous production process of efficient aliphatic concrete water reducing agent Download PDF

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Publication number
CN100430331C
CN100430331C CNB200710023174XA CN200710023174A CN100430331C CN 100430331 C CN100430331 C CN 100430331C CN B200710023174X A CNB200710023174X A CN B200710023174XA CN 200710023174 A CN200710023174 A CN 200710023174A CN 100430331 C CN100430331 C CN 100430331C
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China
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reaction
reducing agent
water reducing
concrete water
continuous production
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Expired - Fee Related
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CNB200710023174XA
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CN101066850A (en
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陆德乾
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JIANGSU HAIRUN CHEMICAL CO Ltd
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JIANGSU HAIRUN CHEMICAL CO Ltd
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Abstract

The present invention is continuous production process of efficient aliphatic concrete water reducing agent, and relates to the industrial production of concrete admixture. The concrete water reducing agent is produced through the first sulfonation reaction of acetone and sodium sulfite solution in vertical tubular reactor and snake-shaped reactor at 68 deg.c and 0.30 MPa to obtain intermediate product; the subsequent condensation reaction of 37 wt% concentration formaldehyde solution and the intermediate product in a tubular reactor at 95 deg.c and 0.30 MPa; and final ageing the condensation reaction product naturally in an ageing tank for 4 hr to obtain the concrete water reducing agent. The production process of the present invention is safe, short, saving in material and low in power consumption.

Description

The continuous production method of efficient aliphatic concrete water reducing agent
Technical field
The present invention relates to concrete admixture chemosynthesis industrial production device field, particularly the continuous production technology of efficient water reducer such as aliphatic hydroxyl sulphonate, melamine system.
Background technology
The synthetic water reducer production industry of chemistry of concrete is nearest 15 years flourish new industries of China, it relies on the foundation of national economy and associated post industry---the pulling of industries such as real estate, traffic, water conservancy, industry, have a bright future, vitality is eternal.But unquestionable is, over 15 years between the evolution of the synthetic water reducer industry of China's chemistry of concrete and the manufacturer mutually in the competition, than capital, only reset fully that reaction capacity enlarges, unlike the raising of technology, light equipment capacity efficient; Overlap into the research of raw material and synthesis route, the gently research and development of synthetic equipment technology.To so far, domestic cement water reducing agent synthesis and production process flow process is homogeneously to adopt that traditional general-purpose equipment---reactor carries out the production of intermittent type list still, and maximum single still volume has been selected for use to 20000 liters.Its production process is that raw material is added in the reactor, makes water reducer through operations such as sulfonation, condensations.As the traditional processing technology flow process that reactor is formed, its major advantage is that operation is simple, but many scarce shaking are arranged: process time is long, production capacity is low, side reaction is many, reaction end is difficult to accurate control, and quality product is difficult for stable.The raw material consumption quota is higher simultaneously, energy consumption is big, environmental pollution is serious.Tank reactor ownership pressurized vessel, job requirement strictnesses such as safety in production, maintenance, management.
Summary of the invention
The object of the invention is to design the continuous production method of the aliphatic concrete water reducing agent that a kind of reaction process safety, time are lacked, economized in raw materials, energy consumption is low.
Technical solution of the present invention is: the sodium sulfite solution of acetone and 60 ℃ is carried out sulfonation reaction earlier in thermal-insulating type vertical pipe reactor and the snakelike reaction tubes of thermal-insulating type, the sulfonation intermediate product is pre-stored in the intermediate equilibria jar, wherein, to keep 68 ± 2 ℃ temperature of reaction, reaction pressure in vertical pipe reactor and snakelike reaction tubes be 0.30MPa to reaction mixture; Be that 37% formaldehyde and sulfonation intermediate product pump into and carry out condensation reaction in the thermal-insulating type reaction tubes again with concentration, wherein, the temperature of reaction of reaction tubes reaction mixture is that 95 ℃, reaction pressure are 0.30MPa; The condensation reaction thing is stored in weather aging after 4 hours in the insulation digestion tank, promptly makes efficient aliphatic concrete water reducing agent.
The invention provides the optimum reaction condition of continuous desirable mixed flow model, mixing and reaction times are adjustable.Can be temperature required according to processing requirement segmentation control reaction.The snakelike reaction tubes of thermal-insulating type vertical pipe reactor and thermal-insulating type in the sulfonation reaction, and the flow model that provides the stack of comparatively ideal piston flow radially to mix diffusion for each elementary reaction material of the reaction tubes in the condensation reaction, to rate of mass transfer, the homogenizing temperature of reaction of reaction system, restrain the system side reaction and create and be suitable for favourable condition.Also can be according to processing requirement at the reaction system a certain conversion zone in section or the system flow sometime, can change operating mode on space-time flexibly provides and reacts required suitable pressure.
The whole synthesis process of the present invention is closed circuit operation, cleaner production, non-environmental-pollution, equipment safety in operation height, has the production serialization, equipment miniaturization, easy to operate, the reaction dynamic response is fast and reaction conditions that be easy to operation is set is under the dynamic stability operating mode labour productivity height, energy-conservation economize on electricity, productive rate height, constant product quality.The synthesis system that adopts this technical process to build up, facility investment is few, the system equipment compactness, floor space is little, need not tall and big factory building and steel construction, only needs the single-storey factory building of height about 5M.
In addition, Gu in order effectively to improve required reaction interface between liquid---liquid, liquid---two-phase and the multiple phase reactant, reaction pump adopts the high-speed centrifugal reaction pump.
In order to make centrifugal reaction pump in reactant normally operation under the temperature of reaction condition, physical attribute according to acetone, formaldehyde, must guarantee that the import thing liquid of centrifugal reaction pump is the malleation operating mode, acetone, formaldehyde solution have adopted has the small-sized impeller pump malleation of certain discharge head to pump into centrifugal reaction pump.The mass velocity of acetone is 300Kg/h, and the mass velocity of sodium sulfite solution is 1800Kg/h.
In order effectively to prevent generation of static electricity, to gather, and the acetone that helps low discharge is scattered in the sodium sulfite solution of big relatively flow better, and the acetone pipe head is than the close pump impeller center of sodium sulfite solution pipeline.
For the ease of control reaction temperature, the thermal-insulating type vertical pipe reactor is provided with insulation jacket, charges into steam or hot water in interlayer.
Simultaneously, the snakelike reaction tubes of thermal-insulating type is provided with insulation jacket, charges into steam or hot water in interlayer.
In order to guarantee that reactant participates in the required appropriate molar ratios of reaction, the mass velocity with 2100Kg/h and 800Kg/h pumps into intermediate reaction liquid and formaldehyde solution to the thermal-insulating type reaction tubes respectively.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
With the production of aliphatic hydroxyl sulphonate high efficiency water reducing agent is example.
The sodium sulfite solution and the acetone that are warming up to 60 ℃ are pumped into the centrifugal reaction pump that corrosion resistant material is made as 304 materials with the small flow centrifugal pump through under meter simultaneously with 1800Kg/h and 300Kg/h mass velocity respectively, acetone pipe outlet exchange premium pump impeller center.
Reaction mass the high-speed stirring of pump impeller disperse and reaction under squeeze into and have steam (or hot water) chuck, be built-in with the corrosion resistant material that mixes components and parts vertical pipe reactor as 304 materials, there are steam (hot water) chuck, inwall to have the snakelike reaction tubes of 304 materials of inner spiral groove outside entering then, proceed liquid---liquid phase reaction, keep 68 ± 2 ℃ of temperature of reaction, control reaction pressure 0.30MPa.
When reaction solution is full of intermediate equilibria jar 1/3rd liquid levels, start No. 2 reaction pump, the formaldehyde of intermediate reaction liquid and 37% is entered this pump and the serial connection reaction tubes is proceeded sulfonation and condensation consecutive reaction with the mass velocity of 2100Kg/h and 800Kg/h through under meter respectively, temperature of reaction system when adjusting and the outlet of maintenance reaction tubes is controlled reaction pressure 0.30MPa at 95 ℃.Reaction solution enters under the digestion tank (1) that has the adiabator parcel or (2) natural thermal insulation condition aging 4 hours by reaction tubes outlet, and the sampling and measuring flowing degree of net paste of cement meets quality standard.The liquid product volume was at 1.2~2.0% o'clock, and water-reducing rate is 18%~30%.With other admixtures good intermiscibility is arranged, can be used, make the composite product of various functional types.
2.9 tons/hour of this Production Flow Chart production capacities, continuous production can be produced 60 tons of water aqua type aliphatic hydroxyl sulphonate high efficiency water reducing agents daily, and the every quality index of product can reach the advanced index of domestic product of the same type.
Need equipment to drop into 250,000 yuan by 20000 tons of scales of above technology annual capacity, be about 20% of same industrial scale traditional batch single kettle type synthesis process flow process investment cost, the energy consumption power consumption only is about 30% of a same industrial scale traditional batch single kettle type synthesis process flow process.

Claims (6)

1, the continuous production method of efficient aliphatic concrete water reducing agent, it is characterized in that the sodium sulfite solution of acetone and 60 ℃ is carried out sulfonation reaction earlier in thermal-insulating type vertical pipe reactor and the snakelike reaction tubes of thermal-insulating type, the sulfonation intermediate product is pre-stored in the intermediate equilibria jar, wherein, to keep 68 ± 2 ℃ temperature of reaction, reaction pressure in vertical pipe reactor and snakelike reaction tubes be 0.30MPa to reaction mixture; Be that 37% formaldehyde and sulfonation intermediate product pump into and carry out condensation reaction in the thermal-insulating type reaction tubes again with concentration, wherein, the temperature of reaction of reaction tubes reaction mixture is that 95 ℃, reaction pressure are 0.30MPa; The condensation reaction thing is stored in weather aging after 4 hours in the insulation digestion tank, promptly makes efficient aliphatic concrete water reducing agent.
2, according to the continuous production method of the described efficient aliphatic concrete water reducing agent of claim 1, when it is characterized in that acetone and sodium sulfite solution mix, adopt centrifugal reaction pump to pump into, the mass velocity of acetone is 300Kg/h, and the mass velocity of sodium sulfite solution is 1800Kg/h.
3,, it is characterized in that the acetone pipe head is than the close pump impeller center of sodium sulfite solution pipeline according to the continuous production method of the described efficient aliphatic concrete water reducing agent of claim 2.
4,, it is characterized in that the thermal-insulating type vertical pipe reactor is provided with insulation jacket, charges into steam or hot water in interlayer according to the continuous production method of the described efficient aliphatic concrete water reducing agent of claim 1.
5,, it is characterized in that the snakelike reaction tubes of thermal-insulating type is provided with insulation jacket, charges into steam or hot water in interlayer according to the continuous production method of the described efficient aliphatic concrete water reducing agent of claim 1.
6,, it is characterized in that respectively pumping into intermediate reaction liquid and formaldehyde solution to the thermal-insulating type reaction tubes with the mass velocity of 2100Kg/h and 800Kg/h according to the continuous production method of the described efficient aliphatic concrete water reducing agent of claim 1.
CNB200710023174XA 2007-06-05 2007-06-05 Continuous production process of efficient aliphatic concrete water reducing agent Expired - Fee Related CN100430331C (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101885817A (en) * 2010-07-27 2010-11-17 大连市铭源全科技开发有限公司 Aliphatic sulfonate water reducing agent prepared from magnetized water
CN102745934A (en) * 2011-04-27 2012-10-24 江苏尼高科技有限公司 Stepped multiple tank continuous production method of aliphatic water reducer
CN103537241B (en) * 2013-10-16 2015-07-01 北京新奥混凝土集团有限公司 Single-channel tubular reaction device for producing polycarboxylate superplasticizer
CN106396456B (en) * 2016-08-26 2018-07-03 河南科之杰新材料有限公司 A kind of preparation method of aliphatic powder water-reducing agent
CN111992156A (en) * 2020-08-27 2020-11-27 聊城大学 Continuous synthesis method and application of sulfonated ketone-aldehyde condensation compound

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1066448A (en) * 1991-05-08 1992-11-25 中原石油勘探局钻井工程服务公司 The manufacture method of sulphonated acetone formaldehyde polycondensates
CN1704371A (en) * 2004-05-28 2005-12-07 班俊生 High performance water-reducing agent of sulfanilate-sulfonated acetone-formaldehyde condensate and process for making same
CN1821150A (en) * 2006-03-03 2006-08-23 南通华润新材料有限公司 Process for preparing poly carboxylic acid modified fatty water-reducing agent

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1066448A (en) * 1991-05-08 1992-11-25 中原石油勘探局钻井工程服务公司 The manufacture method of sulphonated acetone formaldehyde polycondensates
CN1704371A (en) * 2004-05-28 2005-12-07 班俊生 High performance water-reducing agent of sulfanilate-sulfonated acetone-formaldehyde condensate and process for making same
CN1821150A (en) * 2006-03-03 2006-08-23 南通华润新材料有限公司 Process for preparing poly carboxylic acid modified fatty water-reducing agent

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