CN112999993A - Vortex-spraying two-stage strengthening reactor for preparing polycarboxylate superplasticizer and preparation method - Google Patents

Vortex-spraying two-stage strengthening reactor for preparing polycarboxylate superplasticizer and preparation method Download PDF

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CN112999993A
CN112999993A CN202110180412.8A CN202110180412A CN112999993A CN 112999993 A CN112999993 A CN 112999993A CN 202110180412 A CN202110180412 A CN 202110180412A CN 112999993 A CN112999993 A CN 112999993A
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reactor
raw materials
pipe
spraying
reducing agent
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CN112999993B (en
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马跃飞
高明星
徐江红
张皓
蒋国宝
张小琼
蒋镜昱
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Wulanhaote Shengyishang Concrete Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/26Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/24Macromolecular compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers

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Abstract

The invention discloses a vortex-spraying two-stage strengthening reactor for preparing a polycarboxylate water reducer and a preparation method, wherein the vortex-spraying two-stage strengthening reactor comprises a spraying reactor, a turbofan jet mixer, a fluidization pipeline, a first feeding pipe and a stirrer, wherein the turbofan jet mixer is communicated with the spraying reactor through a connecting pipe; wherein the connection of the fluidization conduit to the injection reactor forms a venturi effect. According to the invention, the diffusion tube with the taper of 3-5 degrees (the flow rate of the raw materials is more than or equal to 25m/s) is utilized, so that the mixed raw materials rotate in a high-speed turbulent flow manner in the diffusion tube, the collision among the raw materials is enhanced, the raw materials are promoted to rapidly generate a polymerization reaction, and the preparation time of the polycarboxylic acid water reducing agent is shortened.

Description

Vortex-spraying two-stage strengthening reactor for preparing polycarboxylate superplasticizer and preparation method
Technical Field
The invention relates to a device for preparing a high-performance concrete admixture and a process for preparing the high-performance concrete admixture, in particular to a vortex spraying two-stage strengthening reactor for preparing a polycarboxylic acid water reducing agent and a preparation method thereof.
Background
The polycarboxylate superplasticizer is the latest concrete superplasticizer at present, has the characteristics of high water reducing rate, low mixing amount, good construction performance and the like, has no pollution in production and application, meets the requirements of national green and environment-friendly products, is advocated by extensive scientific research institutions and production enterprises, and strives for research and development to improve the technical level of production, improve the performance of products, reduce the production cost, save energy and improve the production efficiency.
However, at present, the domestic production process and equipment still continue to use the batch production process for decades, and the single-pot single-batch equipment mainly comprises a reaction pot.
The new development of the admixture technology is introduced from various aspects by the data of Chinese concrete admixture application technical society and the related technical data of Chinese chemical admixture and mineral admixture research and application new development, but the invention recommends and introduces the technical performance of the product and the improvement of the mixture ratio of materials participating in polymerization reaction, and the like. The improvement of the production process and the equipment is reported. The patent number is: CN10294259A, patent name: a method for producing a polycarboxylic acid high-performance water reducing agent by using a tubular reaction device comprises the following steps of: two patents of a single-channel tubular reaction device for producing a polycarboxylate water reducer disclose two devices for producing a polycarboxylate high-performance water reducer. However, when the polycarboxylic acid high performance water reducing agent is prepared in the two devices, the reaction time is long and the efficiency is low because the mixing reaction is carried out in a single-channel self-flowing state, and the dynamic process of the polymerization reaction is not developed and researched, so that the production efficiency cannot be improved and the purpose of saving energy cannot be achieved. Further, "patent numbers are: CN103497285A, patent name: a method for preparing a polycarboxylic acid graft copolymer type efficient superplasticizer by a microwave-assisted method is disclosed in the patent, wherein a microwave radiation device is used for promoting polymerization reaction. However, the microwave devices are composed of a large number of parts, so that microwave components are not easy to control, maintenance is not facilitated, and the cost is high, thereby being not beneficial to popularization in the market.
According to the above-mentioned several prior art descriptions, they do not improve from the theory and practice of the kinetic process of polymerization, only in the selection of material proportion, heating form and temperature control and addition of facilities. The technical data which can improve the chemical reaction engineering technical equipment, save energy and realize fundamental comprehensive performance is not reported at home at present, so that a device for preparing the high-performance polycarboxylate superplasticizer, which can improve the technical level of production, improve the performance of products, reduce the production cost, save energy and improve the production efficiency, becomes a research hotspot at present.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention aims to provide a vortex-spraying two-stage strengthening reactor for preparing a polycarboxylate superplasticizer, which can be used for continuously producing and shortening the preparation time of the polycarboxylate superplasticizer.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a vortex-spraying two-stage strengthening reactor for preparing a polycarboxylate water reducer comprises a spraying reactor, a vortex fan spraying mixer, a fluidization pipeline, a first feeding pipe and a stirrer, wherein the vortex fan spraying mixer is communicated with the spraying reactor through a connecting pipe; wherein, one end of the connecting pipe is connected with the tail end of the turbofan jet mixer, and the other end of the connecting pipe is connected with the head end of the jet reactor; the connection of the fluidisation pipe to the injection reactor creates a venturi effect.
Preferably, the vortex spraying two-stage strengthening reactor further comprises a second feeding pipe arranged on the side wall of the spraying reactor, and a detection hole arranged on the side wall of the turbofan spraying mixer; wherein, unqualified polycarboxylate superplasticizer or partial raw materials enter the injection reactor through a second feeding pipe.
Preferably, the stirrer comprises a turbofan stirrer arranged at the head end of the turbofan jet mixer and positioned inside the turbofan jet mixer, and a rotating shaft connected with the turbofan stirrer; the rotating shaft drives the turbofan stirrer to rotate at a high speed under the driving of the motor and intensively stir and mix the raw materials, and fluid dynamic pressure which is more than or equal to 0.5MPa is formed while the raw materials are mixed.
Preferably, the fluidization pipeline comprises a diffusion pipe which is connected to the tail end of the injection reactor and has a taper of 3-5 degrees, and a straight pipe connected with the diffusion pipe; the device comprises a spray reactor, a diffusion pipe, a straight pipe, a raw material, a primary polycarboxylic acid water reducing agent and a polycarboxylate superplasticizer, wherein the spray reactor is connected with a small port of the diffusion pipe and forms a Venturi effect at the joint, the straight pipe is connected with a large port of the diffusion pipe, the raw material is subjected to a polymerization reaction in the diffusion pipe rapidly to obtain the primary polycarboxylic acid water reducing agent, and the primary polycarboxylic acid water reducing agent is subjected to a polymerization reaction in the straight pipe continuously.
Preferably, the straight pipe has a length L of (80 to 400) × D, and the diffuser pipe has a length L of (30 to 50) × D.
The invention also aims to provide a preparation method of the polycarboxylate superplasticizer, which comprises the following steps:
step 1, raw materials enter a turbofan jet mixer through a first feeding pipe, a stirrer is used for carrying out high-speed rotary mixing on the raw materials in the turbofan jet mixer, and the mixed raw materials are pushed into a jet reactor under the action of fluid dynamic pressure generated by the stirrer;
step 2, the mixed raw materials enter a diffusion tube through a jet reactor, and the raw materials are subjected to a polymerization reaction rapidly in the jet reactor and the diffusion tube to obtain a primary polycarboxylic acid water reducing agent;
step 3, allowing the primary polycarboxylic acid water reducing agent to enter a straight pipe, and continuing to perform polymerization reaction in the straight pipe to obtain a polycarboxylic acid water reducing agent;
and returning part of the raw materials or unqualified polycarboxylate superplasticizer from the second feeding pipe to the injection reactor, and repeating the step 2 and the step 3.
Preferably, the raw materials mixed, stirred and pressurized in the step 1 enter a jet reactor through a connecting pipe at a flow rate of more than or equal to 30 m/s; the flow velocity of the mixed raw materials in the diffusion tube in the step 2 is more than or equal to 25 m/s; and 3, the flow rate of the primary polycarboxylic acid water reducing agent in the straight pipe in the step 3 is more than or equal to 25 m/s.
Compared with the prior art, the invention has the following beneficial effects:
(1) the vortex-spraying two-stage strengthening reactor disclosed by the invention realizes the continuous production of the polycarboxylate superplasticizer, so that the production efficiency of the polycarboxylate superplasticizer is improved, and the preparation cost of the polycarboxylate superplasticizer is reduced. In addition, according to the test analysis in the specification of the application, the polycarboxylate water reducer prepared by the vortex-spraying two-stage strengthening reactor has good stability (according to the record in table 2, the polycarboxylate water reducer prepared by the vortex-spraying two-stage strengthening reactor has small performance fluctuation after being placed for half a year and is subjected to test analysis on the performance of the polycarboxylate water reducer).
(2) In the invention, the strongly stirred and mixed raw materials are subjected to polymerization reaction in a fluidized pipeline to generate the polycarboxylic acid water reducing agent. The taper of the diffusion tube is 3-5 degrees, the flow rate of the raw materials in the diffusion tube is more than or equal to 25m/s, so that the raw materials after intensive stirring and mixing rotate in the diffusion tube in a high-speed turbulent flow manner, collision among the raw materials is enhanced, the raw materials are promoted to rapidly generate a polymerization reaction, and the preparation time of the polycarboxylic acid water reducing agent is shortened. And a straight pipe which is connected with the large port of the diffusion pipe and has the length L of (80-400) multiplied by D is a place for continuing the polymerization reaction, and finally the polycarboxylate superplasticizer is obtained.
Therefore, the diffusion pipe and the straight pipe in the invention ensure that the raw materials can complete the polymerization reaction according to the requirements of chemical reaction engineering kinetics, and finally the polycarboxylic acid water reducing agent in the invention is obtained. According to practical experience, the pipeline of the whole turbojet two-stage strengthening reactor is generally free from phenomena of stagnation, implosion and the like in the polymerization reaction process, the production efficiency of the polycarboxylate superplasticizer is further improved, and the preparation cost of the polycarboxylate superplasticizer is reduced.
(3) The jet reactor of the invention is connected with the small port of the diffusion pipe and forms a Venturi effect at the connection position. On one hand, the formed Venturi effect can promote the unqualified polycarboxylate superplasticizer to enter the spraying reactor through the second feeding pipe; on the other hand, the catalyst, initiator, reducing agent and chain transfer agent for polymerization may be fed into the injection reactor through the second feed line. And the formed Venturi effect can also promote the materials (unqualified polycarboxylate superplasticizer or partial raw materials) entering from the second feeding pipe and the mixed raw materials from the turbofan jet mixer to be fully and uniformly mixed, and promote the collision between the strongly stirred and mixed raw materials, thereby being beneficial to fully carrying out the polymerization reaction and improving the polymerization reaction rate. In addition, the unqualified polycarboxylate water reducer is directly fed into the injection reactor through the second feeding pipe, so that compared with the traditional unqualified polycarboxylate water reducer which needs to be subjected to polymerization from the beginning, the time for preparing the qualified polycarboxylate water reducer from the unqualified polycarboxylate water reducer is shortened, and the production efficiency of the polycarboxylate water reducer is improved.
(4) Compared with the single-pot single-batch intermittent production equipment for the polycarboxylate superplasticizer in the prior art, the equipment has the advantages of small occupied area and reduction of the preparation cost of the polycarboxylate superplasticizer. Compared with single-pot single-batch intermittent production of the polycarboxylate water reducer, the vortex-spraying two-stage strengthening reactor can be used for continuous production (no blockage phenomenon exists in the production process), and the polymerization reaction time of the polycarboxylate water reducer is shortened to dozens of minutes (the length of each batch of polycarboxylate water reducer produced by single-pot single-batch intermittent production is 5-6 hours); therefore, the efficiency of the polymerization reaction is greatly improved, the efficiency is improved by 8-10 times according to actual experience calculation, and the effect of large-scale production of small equipment is realized.
Drawings
FIG. 1 is a schematic structural view of a turbojet dual-stage enhanced reactor according to the present invention;
FIG. 2 is a schematic view of the structure of the present invention in which the stirrer is disposed at the head end of the turbofan jet mixer;
FIG. 3 is a schematic diagram of a preparation process of a carboxylic acid water reducing agent in the present invention;
wherein, the names corresponding to the reference numbers are:
1-turbofan jet mixer, 2-jet reactor, 3-first feeding pipe, 4-second feeding pipe, 5-detection hole, 6-stirrer, 7-turbofan stirrer, 8-connecting pipe, 9-rotating shaft, 10-fluidization pipeline, 11-diffusion pipe, 12-straight pipe, 13-detection tank, 14-detection system, 15-product tank and 16-reflux device.
Detailed Description
1. The Chinese names corresponding to English abbreviations of the substances in the invention are shown in Table 1:
TABLE 1 Chinese name corresponding to English abbreviation of each substance
Figure BDA0002941320820000051
Figure BDA0002941320820000061
2. The polycarboxylic acid water reducing agent is prepared from polyether macromonomer, unsaturated organic acid ester and functional monomer under the action of a catalyst, an initiator, a reducing agent and a chain transfer agent.
Wherein the polyether macromonomer is HPEG or TPEG;
the unsaturated organic acid is MAA or AA;
the unsaturated organic acid ester is HEA or HPA;
the functional monomer is SMAS, AM or HEDP;
the catalyst is as follows: DMAP;
the initiator is as follows: APS, H2O2
The reducing agent is: vc;
the chain transfer agent is: MPA.
Examples
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred devices or elements must have a specific orientation or be constructed and operated in a specific orientation, and thus, they should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and the like are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected; of course, mechanical connection and electrical connection are also possible; alternatively, they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Example 1
As shown in fig. 1, the two-stage intensive reactor of the present invention includes a turbofan jet mixer 1, a jet reactor 2, a first feeding pipe 3, a second feeding pipe 4, a detection hole 5, a connection pipe 8, a fluidization pipe 10, and a stirrer 6. Specifically, the turbofan jet mixer 1 is communicated with the jet reactor 2 through a connecting pipe 8, a fluidization pipeline 10 is connected to the tail end of the jet reactor 2, the first feeding pipe 3 is connected to the head end of the turbofan jet mixer 1, and the stirrer 6 is arranged at the head end of the turbofan jet mixer 1; the second feeding pipe 4 is provided on the side wall of the injection reactor 2, and the sensing hole 5 is provided on the side wall of the turbofan injection mixer 1. Wherein, one end of the connecting pipe 8 is connected with the tail end of the turbofan jet mixer 1, and the other end is connected with the head end of the jet reactor 2; the connection of the fluidization conduit 10 to the injection reactor 2 forms a venturi effect; and part of raw materials or unqualified polycarboxylate superplasticizers are fed into the injection reactor 2 through the second feeding pipe 4 and undergo polymerization reaction in the fluidized pipeline 10 to generate the polycarboxylate superplasticizers.
Specifically, the raw materials enter the turbofan jet mixer 1 through the first feeding pipe 3, the stirrer 6 intensively stirs and mixes the raw materials in the turbofan jet mixer 1, and generates a fluid dynamic pressure of not less than 0.5MPa while mixing the raw materials, so that the mixed raw materials are pushed into the jet reactor 2, and then the mixed raw materials enter the fluidization pipeline 10 for polymerization reaction to obtain the polycarboxylic acid water reducer. Wherein, the mixed raw materials enter the jet reactor 2 at a flow rate of more than or equal to 30m/s, and the strongly stirred and mixed raw materials are also in violent collision in the jet reactor 2 all the time.
In addition, the unqualified polycarboxylate superplasticizer or part of raw materials (such as an initiator, a catalyst, a reducing agent, chain transfer and functional monomers) enters the injection reactor 2 through the second feeding pipe 4 under the action of a Venturi effect formed at the joint of the fluidized pipeline 10 and the injection reactor 2, and the polymerization reaction is continued in the fluidized pipeline 10, so that the polycarboxylate superplasticizer is obtained.
As shown in fig. 1 and 2, the stirrer 6 includes a turbofan stirrer 7 and a rotating shaft 9. Specifically, the turbofan stirrer 7 is disposed at the head end of the turbofan jet mixer 1 and located in the turbofan jet mixer 1, and the rotating shaft 9 is connected to the turbofan stirrer 7. The rotating shaft 9 drives the turbofan stirrer 7 to rotate at a high speed under the driving of the motor, so that the turbofan stirrer 7 mixes the raw materials, and forms a fluid dynamic pressure of not less than 0.5MPa while mixing, and the operating principle of the turbofan stirrer 7 is the same as that of a gas turbine.
As shown in fig. 1 and 2, the fluidization conduit 10 includes a diffuser pipe 11 and a straight pipe 12. Specifically, the diffuser 11 is connected to the tail end of the injection reactor 2, and the taper of the diffuser 11 is 3-5 ° and the length L is (30-50) × D; the straight pipe 12 is connected with the diffusion pipe 11, and the length L of the straight pipe 12 is (80-400) multiplied by D; wherein, the small port of the diffuser pipe 11 is connected with the injection reactor 2 and forms a Venturi effect at the connection part, and the large port of the diffuser pipe 11 is connected with the straight pipe 12. The length calculation formulas for diffuser pipe 11 and straight pipe 12 in this example are both the diameter of straight pipe 12.
Specifically, the strongly stirred and mixed raw materials rotate in a high-speed violent turbulent flow shape in the diffusion tube 11 and collide with each other, and the flow speed of the mixed raw materials in the diffusion tube is more than or equal to 25m/s, so that the raw materials are promoted to rapidly carry out polymerization reaction to obtain a primary polycarboxylic acid water reducing agent; the primary polycarboxylic acid water reducing agent continues to carry out polymerization reaction in the straight pipe 12, and the flow rate of the primary polycarboxylic acid water reducing agent in the straight pipe is more than or equal to 25m/s, so that the polycarboxylic acid water reducing agent is obtained.
Example 2
As shown in fig. 3, this embodiment provides a system for preparing a polycarboxylate water reducer, which includes the vortex-spraying two-stage strengthening reactor described in embodiment 1, a detection tank 13 connected to the tail end of the straight pipe 12 in the vortex-spraying two-stage strengthening reactor, a product tank 15 connected to the detection tank 13, a reflux unit 16 connected to the detection tank 13, and a detection system 14 for detecting the pH, density, and viscosity of the polycarboxylate water reducer in the detection tank 13. In this embodiment, the polycarboxylate water reducing agent in the detection tank 13 is detected by the detection system 14, and the unqualified polycarboxylate water reducing agent is returned to the injection reactor 2 from the second feeding pipe 4 through the reflux device 16, and the polymerization reaction is rapidly carried out in the diffusion pipe 11, and the polymerization reaction is continued in the straight pipe 12; the polycarboxylate water reducing agent in the detection tank 13 is detected by the detection system 14, and the qualified polycarboxylate water reducing agent flows into the product tank 15.
Example 3
On the basis of embodiment 1 and embodiment 2, this embodiment provides a preparation method of a polycarboxylic acid water reducing agent, which specifically includes the following steps:
step 1, from 1.5kg of H2O2(H2O227.5%) and 19kg of pure water were added to the mixture a.
And 2, starting a turbofan jet mixer, simultaneously adding the mixture A, the mixture B, the mixture C, the mixture D and the mixture E into the turbofan jet mixer through a first feeding hole within 30-40 minutes, and intensively stirring and mixing the mixture by using a stirrer, wherein the temperature is controlled to be less than or equal to 45 ℃. The mixed raw materials enter a jet reactor under the push of fluid dynamic pressure which is formed by high-speed rotation of a stirrer and is more than or equal to 0.5 MPa;
wherein, the mixture A is obtained by mixing 340kg of HPEG with 260kg of pure water;
the B mixture is obtained by mixing 39kg of AA with 34kg of pure water;
the mixture C is obtained by mixing 5kg of SMAS and 30kg of pure water;
the mixture D was obtained by mixing 5kg of HEA with 10kg of purified water;
the E mixture was obtained by mixing 2.4kg of APS, 0.6kg of Vc and 0.8kg of MPA with 50kg of pure water.
Step 3, the mixed raw materials enter a jet reactor at a flow rate of more than or equal to 30m/s, then enter a diffusion tube and rotate in the diffusion tube in a high-speed violent turbulent flow shape and collide with each other, so that the raw materials are promoted to rapidly carry out polymerization reaction, and the primary polycarboxylic acid water reducing agent is obtained; the primary polycarboxylic acid water reducing agent continues to carry out polymerization reaction in the straight pipe, so that the polycarboxylic acid water reducing agent is obtained; wherein the flow rate of the raw materials in the diffusion tube is more than or equal to 25 m/s; the flow rate of the primary polycarboxylic acid water reducing agent in the straight pipe is more than or equal to 25 m/s.
And 4, according to the feedback of the detection system, adding 261kg of pure water through the first feeding hole to adjust the solid content in the polycarboxylate superplasticizer obtained through continuous polymerization to be 40 +/-1%.
And 5, on the basis of the step 4, adding 40kg of NaOH with the mass concentration of 32% into the polycarboxylate superplasticizer obtained by continuous polymerization according to the feedback of the detection system to adjust the pH value of the polycarboxylate superplasticizer to 5-5.5 to obtain polycarboxylate superplasticizer (PCE) mother liquor, and enabling the PCE mother liquor to flow into a product tank, thereby obtaining the final polycarboxylate superplasticizer product.
Samples 1 and 2 with the mass of 1kg are taken from the polycarboxylate water reducer product prepared in the embodiment, wherein the sample 1 is detected according to the GB8076-2008 standard in the current month, the sample 2 is detected according to the GB8076-2008 standard after being placed for half a year, and the detection results of the samples 1 and 2 are shown in Table 2.
Example 4
On the basis of embodiment 1 and embodiment 2, this embodiment provides a preparation method of a polycarboxylic acid water reducing agent, which specifically includes the following steps:
step 1, starting a turbofan jet mixer, adding the mixture A, the mixture B, the mixture C, the mixture D, the mixture E and 0.8kg of low-temperature catalyst DMAP (4-dimethylaminopyridine) into the turbofan jet mixer through a first feeding hole at the same time within 30-40 minutes, mixing, stirring and pressurizing the mixture through a stirrer, and controlling the temperature to be less than or equal to 45 ℃. The mixed raw materials enter a jet reactor under the push of fluid dynamic pressure which is formed by high-speed rotation of a stirrer and is more than or equal to 0.5 MPa;
wherein, the mixture A is obtained by mixing 340kg of HPEG (methallyl alcohol polyoxyethylene ether) and 260kg of pure water;
the B mixture is obtained by mixing 42kg of AA with 30kg of pure water;
the mixture C is prepared by mixing 5kg of HPA and 30kg of pure water;
the mixture D is obtained by mixing 5kg of SMAS and 30kg of pure water;
the E mixture was obtained by mixing 2.4kg of APS, 0.6kg of Vc and 0.8kg of MPA (mercaptopropionic acid) with 50kg of pure water.
Step 2, the mixed raw materials enter a jet reactor at a flow rate of more than or equal to 30m/s, then enter a diffusion tube and rotate in the diffusion tube in a high-speed violent turbulent flow shape and collide with each other, so that the raw materials are promoted to rapidly carry out polymerization reaction, and the primary polycarboxylic acid water reducing agent is obtained; the primary polycarboxylic acid water reducing agent continues to carry out polymerization reaction in the straight pipe, so that the polycarboxylic acid water reducing agent is obtained; wherein the flow rate of the raw materials in the diffusion tube is more than or equal to 25 m/s; the flow rate of the primary polycarboxylic acid water reducing agent in the straight pipe is more than or equal to 25 m/s.
And 3, according to the feedback of the detection system, adding 261kg of pure water through the first feeding hole to adjust the solid content in the polycarboxylate superplasticizer obtained through continuous polymerization to be 40 +/-1%.
And 4, on the basis of the step 4, adding NaOH with the mass concentration of 32% into the polycarboxylate water reducer obtained by continuous polymerization according to the feedback of the detection system to adjust the pH value of the polycarboxylate water reducer to 5-5.5 to obtain polycarboxylate water reducer (PCE) mother liquor, and enabling the PCE mother liquor to flow into a product tank, thereby obtaining the final polycarboxylate water reducer product.
Sample 3 with the mass of 1kg is taken from the polycarboxylate superplasticizer product prepared in the embodiment, and the sample 3 is detected according to the GB8076-2008 standard after being placed for half a year, and the detection data are shown in Table 2.
And (3) testing and analyzing:
samples 1, 2, 3 and a standard sample (the standard sample is PCE of shanghai solid-enhanced chemical technology ltd, wherein the model of the PCE is GJ-M40, and the solid content is 40%), were tested according to GB8076-2008, and the test results are shown in table 2.
TABLE 2 test results of the respective samples
Figure BDA0002941320820000111
As can be seen from Table 2, the polycarboxylate water reducer prepared by the vortex-spraying two-stage strengthening reactor provided by the invention has small performance fluctuation after 6 months of storage, which indicates that the polycarboxylate water reducer prepared by the vortex-spraying two-stage strengthening reactor provided by the invention has stable quality.
In summary, the present invention solves the technical deficiencies of the prior art. The invention connects the turbofan jet mixer, the jet reactor and the fluidization pipeline; on one hand, the unqualified polycarboxylate superplasticizer is promoted to enter the jet reactor through the second feeding pipe by utilizing the Venturi effect formed at the joint of the fluidization pipeline and the jet reactor; on the other hand, the catalyst, initiator, reducing agent and chain transfer agent for polymerization may be fed into the injection reactor through the second feed line. The mixed raw materials are violently collided in the injection reactor by utilizing the Venturi effect, and simultaneously, the diffusion tube with the taper of 3-5 degrees (the flow velocity of the raw materials in the diffusion tube is more than or equal to 25m/s) rotates in a high-speed turbulence manner in the diffusion tube, so that the collision among the raw materials is enhanced, the raw materials are promoted to carry out high-speed polymerization reaction, and the primary polycarboxylic acid water reducing agent is obtained, so that the preparation time of the polycarboxylic acid water reducing agent is shortened.
The foregoing is only a partial embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (7)

1. The vortex spraying two-stage strengthening reactor for preparing the polycarboxylate water reducer is characterized by comprising a spraying reactor (2), a vortex fan spraying mixer (1) communicated with the spraying reactor (2) through a connecting pipe (8), a fluidization pipeline (10) which is connected to the tail end of the spraying reactor (2) and used for carrying out polymerization reaction on raw materials to obtain the polycarboxylate water reducer, a first feeding pipe (3) connected to the head end of the vortex fan spraying mixer (1), and a stirrer (6) which is arranged at the head end of the vortex fan spraying mixer (1) and used for intensively stirring and mixing the raw materials and generating fluid dynamic pressure; wherein, one end of the connecting pipe (8) is connected with the tail end of the turbofan jet mixer (1), and the other end is connected with the head end of the jet reactor (2); the connection of the fluidization conduit (10) to the injection reactor (2) forms a venturi effect.
2. The turbojet two-stage strengthening reactor for preparing the polycarboxylate superplasticizer according to claim 1, further comprising a second feeding pipe (4) arranged on the side wall of the jet reactor (2), and a detection hole (5) arranged on the side wall of the turbofan jet mixer (1); wherein the unqualified polycarboxylate superplasticizer or part of raw materials enter the injection reactor (2) through a second feeding pipe (4).
3. The vortex spraying two-stage strengthening reactor for preparing the polycarboxylate superplasticizer according to the claim 2, wherein the stirrer (6) comprises a vortex fan stirrer (7) arranged at the head end of the vortex fan jet mixer (1) and positioned inside the vortex fan jet mixer (1), and a rotating shaft (9) connected with the vortex fan stirrer (7); the rotating shaft (9) is driven by the motor to drive the turbofan stirrer (7) to rotate at a high speed and intensively stir and mix the raw materials, and fluid dynamic pressure which is more than or equal to 0.5MPa is formed while the raw materials are mixed.
4. The turbojet two-stage strengthening reactor for preparing water reducing agents of polycarboxylic acids according to claim 3, characterized in that the fluidization pipeline (10) comprises a diffusion pipe (11) which is connected to the tail end of the ejector reactor (2) and has a taper of 3-5 degrees, and a straight pipe (12) connected with the diffusion pipe (11); the device comprises a spray reactor (2), a diffusion pipe (11), a raw material and a straight pipe (12), wherein the spray reactor (2) is connected with a small port of the diffusion pipe (11) and forms a Venturi effect at the joint, the straight pipe (12) is connected with a large port of the diffusion pipe (11), the raw material is subjected to a polymerization reaction in the diffusion pipe (11) rapidly to obtain a primary polycarboxylic acid water reducing agent, and the primary polycarboxylic acid water reducing agent is subjected to a polymerization reaction in the straight pipe (12) continuously to obtain a polycarboxylic acid water reducing agent.
5. The turbojet two-stage strengthening reactor for preparing water reducing agents of polycarboxylic acids according to claim 4, wherein the straight pipe (12) has a length L of (80-400) x D, and the diffuser pipe (11) has a length L of (30-50) x D.
6. A method for preparing a polycarboxylate water reducer is characterized in that the method for preparing the polycarboxylate water reducer by using the turbojet two-stage strengthening reactor disclosed by claims 1-5 specifically comprises the following steps:
step 1, raw materials enter a turbofan jet mixer through a first feeding pipe, a stirrer is used for carrying out high-speed rotary mixing on the raw materials in the turbofan jet mixer, and the mixed raw materials are pushed into a jet reactor under the action of fluid dynamic pressure generated by the stirrer;
step 2, the mixed raw materials enter a diffusion tube through a jet reactor, and the raw materials are subjected to a polymerization reaction rapidly in the jet reactor and the diffusion tube to obtain a primary polycarboxylic acid water reducing agent;
step 3, allowing the primary polycarboxylic acid water reducing agent to enter a straight pipe, and continuing to perform polymerization reaction in the straight pipe to obtain a polycarboxylic acid water reducing agent;
and returning part of the raw materials or unqualified polycarboxylate superplasticizer from the second feeding pipe to the injection reactor, and repeating the step 2 and the step 3.
7. The method for preparing the polycarboxylate superplasticizer according to claim 6, wherein the raw materials mixed, stirred and pressurized in the step 1 enter a jet reactor through a connecting pipe at a flow rate of more than or equal to 30 m/s; the flow velocity of the mixed raw materials in the diffusion tube in the step 2 is more than or equal to 25 m/s; and 3, the flow rate of the primary polycarboxylic acid water reducing agent in the straight pipe in the step 3 is more than or equal to 25 m/s.
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