CN112844250A - Preparation process of water reducing agent for concrete - Google Patents
Preparation process of water reducing agent for concrete Download PDFInfo
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- CN112844250A CN112844250A CN202110055531.0A CN202110055531A CN112844250A CN 112844250 A CN112844250 A CN 112844250A CN 202110055531 A CN202110055531 A CN 202110055531A CN 112844250 A CN112844250 A CN 112844250A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
- B01J8/004—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor by means of a nozzle
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/082—Controlling processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/087—Heating or cooling the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00176—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles outside the reactor
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Abstract
The invention relates to the technical field of concrete, in particular to a preparation process of a water reducing agent for concrete, which comprises the steps of clean blowing, feeding and mixing, curing in a kettle and finished product discharge; the loop reactor used in the method comprises a kettle body and a controller; because the reaction raw materials are inflammable, explosive and highly toxic ethylene oxide gas, the reaction process needs to be precisely controlled, so that potential safety hazards are avoided, and the preparation efficiency is limited; therefore, the heat exchanger is matched with a pipeline arranged on the kettle body, heat generated by addition reaction of the initiator and the ethylene oxide is timely discharged, the initiator reacts with the ethylene oxide in the gas guide tube by using the injection cylinder at the top of the kettle body, the negative pressure value of the gas guide tube at the top of the kettle body is changed, the reaction quantity of the ethylene oxide is adjusted accordingly, and the control on the synthetic state of the polyether macromonomer is achieved by adjusting the circulating pump through the controller, so that the preparation effect of the water reducing agent for concrete is improved.
Description
Technical Field
The invention relates to the technical field of concrete, in particular to a preparation process of a water reducing agent for concrete.
Background
As a main building material in the world, the performance index of concrete is greatly influenced by the water reducing agent. The polycarboxylate superplasticizer is used as a new generation superplasticizer with the best use effect at present, and is applied to concrete for railways, rail transit and other buildings in a large scale; in recent years, as a raw material carrier which is necessary to be adopted for producing the polycarboxylate superplasticizer, the polycarboxylate superplasticizer polyether macromonomer is rapidly researched and developed in China and even in the world, and becomes the mainstream of research and application of the polycarboxylate superplasticizer.
The production process of the raw material carrier of the polyether macromonomer adopted in the production of the polycarboxylate superplasticizer belongs to intermittent strong exothermic reaction, the product has high viscosity and is easy to block reaction equipment, meanwhile, the reaction process of the flammable, explosive and highly toxic ethylene oxide gas in the reaction raw materials needs to be precisely controlled, so that the potential safety hazard is avoided, and the preparation efficiency is limited.
Some technical schemes related to the preparation process of the water reducing agent for concrete also appear in the prior art, for example, a Chinese patent with the application number of 2017113363064 discloses a modified concrete water reducing agent and a preparation method thereof, wherein the water reducing agent is prepared from the following raw materials in parts by weight: 350-365 parts of methyl allyl polyoxyethylene ether, 55-60 parts of modified beta-sodium naphthalene sulfonate, 25-30 parts of methacrylic acid, 1.2-2.0 parts of isopropanol, 3.8-4.2 parts of 30% hydrogen peroxide and 0.5-0.8 part of tetrabutyl titanate; according to the technical scheme, the production cost is reduced while the environmental pollution is reduced by adding the modified sodium naphthalene sulfonate. The preparation process is simple, the synthesized water reducing agent has high water reducing rate and good fluidity and slump retention capacity, the impermeability of concrete is improved, the strength, hardness and density of the concrete are enhanced, and meanwhile, the prepared water reducing agent has good stability and long storage time; however, the technical scheme does not solve the problem that the sodium naphthalenesulfonate in the raw material of the water reducer is in a violent reaction state during the reaction, so that the reaction rate is not convenient to control, and the application effect of preparing the water reducer is weakened.
In view of the above, in order to overcome the technical problems, the invention provides a preparation process of a concrete water reducing agent, which adopts a special preparation process of the concrete water reducing agent, and solves the technical problems.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides a preparation process of a water reducing agent for concrete, which comprises the steps of timely discharging heat generated by addition reaction of an initiator and ethylene oxide by matching a pipeline arranged on a kettle body through an arranged heat exchanger and utilizing an injection cylinder at the top of the kettle body to react the initiator and the ethylene oxide in an air guide pipe, adjusting the initial amount in a loop pipe through a circulating pump, feeding back the initial amount to the injection cylinder to change the flow rate, causing the negative pressure value at the air guide pipe at the top of the kettle body to change, adjusting the reaction amount of the ethylene oxide, and further adjusting the circulating pump through a controller to control the synthetic state of a polyether macromonomer, thereby improving the preparation effect of the water reducing agent for concrete.
The invention relates to a preparation process of a water reducing agent for concrete, which comprises the following steps:
s1, clean purging: purging nitrogen into a loop reactor for preparing the polyether macromonomer through a gas cylinder to ensure that air in a pipeline is discharged and filled with the nitrogen, and starting an electric blanket on the outer wall of the kettle body to keep the temperature of the electric blanket at 15-25 ℃;
s2, feeding and mixing: after the cleaning treatment of the loop reactor in the S1 is finished, the ethylene oxide in the storage bin is communicated with the kettle body of the loop reactor through the air duct, the initiator pre-filled at the bottom of the kettle body is pumped out through the loop pipe, the temperature is controlled at 24-32 ℃ through the external heat exchange pipe, and then the temperature is controlled to the injection cylinder of the loop reactor, the initiator is introduced into the kettle body through the injection cylinder at the top of the kettle body and is mixed with the ethylene oxide input by the air duct, wherein the initiator is ethylene glycol containing active hydrogen;
s3, curing in a kettle: in the reaction process of the S2 kettle body, the circulating initiator carries the catalyst filled in the initiator into the kettle body when passing through the heat exchange tube, the initiator and ethylene oxide are subjected to addition polymerization reaction to generate a polyether macromonomer, and a mixed liquid phase in the kettle body is circulated through the heat exchange tube by utilizing a loop tube to ensure the sufficient reaction between the initiator and the added ethylene oxide;
s4, finished product discharge: after the reaction is carried out in the kettle body for 120min in S3, controlling the state of an initiator in the kettle body in the reaction process to be in 10-15min intermittent operation, finally introducing nitrogen to purge the residual ethylene oxide in the pipeline of the loop reactor, and discharging the polyether macromonomer prepared in the kettle body from the bottom to be used as a raw material carrier of the polycarboxylic acid water reducing agent;
wherein the loop reactor described in S1-S4 comprises a kettle body and a controller; the top of the kettle body is provided with an injection cylinder, and the injection cylinder is communicated with the bottom of the kettle body through a loop pipe; the loop pipe is also internally provided with a heat exchange pipe which is used for conducting the heat of the fluid inside the heat exchange pipe; a circulating pump is also arranged on a pipeline at the top of the heat exchange pipe, and the circulating pump pumps and circulates the fluid in the kettle body through the pipeline; the outer wall of the kettle body is also wrapped with an electric blanket, the top of the kettle body is provided with an annular opening, and the bottom of the kettle body is also provided with a discharge opening; the annular opening of the kettle body is positioned on the circumferential direction of the injection cylinder and is provided with a communicated air guide pipe, the tail end of the air guide pipe is provided with a stock bin and an air bottle which are connected in parallel, and ethylene oxide and nitrogen are respectively stored in the stock bin and the air bottle; the pipeline of the kettle body is provided with an electromagnetic valve for controlling on-off, and the electromagnetic valve and the circulating pump operate under the regulation of the controller;
in the prior art, a polyether macromonomer raw material carrier is adopted in production of a polycarboxylate superplasticizer, the production process belongs to intermittent strong exothermic reaction, the product has high viscosity, and is easy to block reaction equipment, meanwhile, the reaction process of the combustible, explosive and highly toxic ethylene oxide gas in the reaction raw materials needs to be precisely controlled, so that potential safety hazards are avoided, and the preparation efficiency is limited;
therefore, the invention makes the added reacted ethylene oxide and the initiator perform mixed reaction inside the kettle body through the pipeline arranged in the loop reactor, the heat in the reaction process is timely discharged through the heat exchange pipe arranged in the loop pipe between the gas guide pipe and the loop pipe, the electric blanket on the outer wall of the kettle body is used for reducing the heat fluctuation range in the reaction process, the content of free ethylene oxide in the kettle body in the reaction process is reduced after the gas guide pipe is blown with nitrogen for purging, simultaneously the catalyst in the heat exchanger is mixed by the initiator driven by the circulating pump, and then the mixture is converted into high-speed fluid through the jet pipe to perform the synthesis of the polyether macromonomer in the kettle body, and local negative pressure is generated in the top area of the kettle body to carry out the ethylene oxide gas in the gas guide pipe, so that the reaction amount of the ethylene oxide is matched with the initial dosage of the mixed catalyst, taking out the prepared polyether macromonomer through a discharge port; the invention utilizes the arranged heat exchanger to match with a pipeline arranged on the kettle body, the heat generated by the addition reaction of the initiator and the ethylene oxide is discharged in time, the initiator reacts with the ethylene oxide in the gas guide tube by utilizing the jet cylinder at the top of the kettle body, the initial amount in the loop pipe is adjusted by the circulating pump, and then the initial amount is fed back to the flow change in the jet cylinder, so that the negative pressure value of the gas guide tube at the top of the kettle body is changed, the reaction amount of the ethylene oxide is adjusted accordingly, and the control on the synthetic state of the polyether macromonomer is achieved by adjusting the circulating pump by the controller, thereby improving the preparation effect of the water reducing agent for concrete.
Preferably, a guide cylinder is arranged between the kettle body and the air guide pipe, and the guide cylinder is used for communicating the annular opening of the kettle body with the air guide pipe; the guide cylinder is sleeved and mounted at the top of the kettle body, a spring is further mounted between the circumferential outer side of the guide cylinder and the kettle body, and an opening is formed in the inner wall of the guide cylinder in the kettle body; the guide cylinder changes the sectional area between the opening and the injection cylinder under the change of the negative pressure generated by the spring and the injection cylinder, and adjusts the flow of ethylene oxide in the gas guide pipe; when the device is used, the controller adjusts the running state of the circulating pump, and further controls the negative pressure value generated by the jet cylinder in the top area of the kettle body, so as to change the reaction rate between the initiator and ethylene oxide in the kettle body; the kettle body is communicated with the air guide pipe through the guide pipe, the opening of the guide pipe in the kettle body is utilized, so that the negative pressure effect generated by the ejection pipe in a smaller fluid state is realized, the opening is further weakened by the spring between the guide pipe and the kettle body, the sectional area of the opening in the kettle body is reduced, the ethylene oxide amount of the air guide pipe entering the kettle body is limited, the free ethylene oxide which is not reacted with the initiator is prevented from being generated in the kettle body, the safety of the preparation process of the kettle is further enhanced, the displacement inertia generated by the guide pipe in the negative pressure increment state at the top of the kettle body is reduced under the condition that the flow of the initiator is gradually increased in the ejection pipe, the buffering effect of the spring on the guide pipe is utilized, the stability of the reaction process in the kettle body is controlled, and the preparation effect of the water reducing agent for concrete is improved.
Preferably, an arc-shaped bulge is further arranged inside the injection cylinder, and the arc-shaped bulge enables the pipe diameter of the injection cylinder to be a symmetrical hyperboloid body; the spraying cylinder is rotatably arranged on the kettle body, and an impeller surrounding the bulge is also arranged on the inner wall of the bottom port of the spraying cylinder; when the circulating pump is used, the circulating pump drives fluid to enter the injection cylinder through the loop pipe, the impulse of the fluid is lost in the loop pipe, and the circulating pump is required to have larger output in order to meet different reaction rates of the injection cylinder on the initiator and the ethylene oxide; through setting up arc arch in spraying a section of thick bamboo inside for fluid is when getting into the cauldron body through spraying a section of thick bamboo, successively through the pipe diameter effect that diminishes earlier then increase in spraying a section of thick bamboo, has played the venturi effect to the fluid in spraying a section of thick bamboo, has increased the velocity of flow of fluid in cauldron body end spraying a section of thick bamboo, has then increased the flow control scope of circulating pump in to spraying a section of thick bamboo, thereby has promoted the preparation effect of water-reducing agent for concrete.
Preferably, the outer wall of the injection cylinder is also provided with a fixed blade, and the edge of the blade is positioned in a gap between the injection cylinder and the guide cylinder; the blades rotate along with the jet cylinder under the action of the impeller, so that the negative pressure effect on the opening part of the guide cylinder is increased; when the device is used, the ethylene oxide in the storage bin enters the kettle body through the air duct, and the amount of the ethylene oxide entering the kettle body can be weakened due to the pipeline of the air duct; through the blades arranged between the injection cylinder and the guide cylinder, the negative pressure value of the fluid in the injection cylinder in the guide cylinder area is further enhanced in an increment state, the amount of ethylene oxide entering the kettle body from the air guide pipe is enhanced, the flow of the initiator in the injection cylinder is met, the reaction rate required by polyether macromonomer preparation is achieved, the stability of ethylene oxide supply in the air guide pipe is maintained, and the preparation effect of the water reducing agent for concrete is improved.
Preferably, the heat exchange tube is also provided with a catalytic cylinder, the catalytic cylinder is communicated into the heat exchange tube through a branch tube, and a catalyst is filled in the catalytic cylinder; the branch pipe is positioned at the bottom of the catalytic cylinder and the heat exchange pipe; when the catalyst is used, the catalyst pre-installed in the heat exchange pipeline enters the kettle body along with the circulating initiator to catalyze the addition reaction between the ethylene oxide and the initiator, and in order to control the speed of the reaction process, the amount of the catalyst entering the kettle body is matched with the flow rate of the initiator in the heat exchange pipe if needed; the catalyst is independently filled through the arranged catalytic cylinder and is arranged on the heat exchange tube, the catalyst in the catalytic cylinder is accumulated to the position of the branch tube on the heat exchange tube under the action of gravity by utilizing the heat generated in the reaction of the initiator and ethylene oxide emitted from the heat exchange tube to maintain the active state temperature of the catalyst in the catalytic cylinder, and the branch tube is positioned at the bottom positions of the catalytic cylinder and the heat exchange tube, so that the flowing initiator drives the amount of the catalyst stripped from the branch tube in the flow change of the flowing initiator entering the heat exchange tube, and the preparation effect of the water reducing agent for concrete is improved.
Preferably, the branch pipe is smaller than the pipe diameter of the heat exchange pipe, and a rotary web plate is further arranged in the branch pipe; the web plate enables the branch pipe to be in a closed state at the port of the heat exchange pipe under the action of gravity, a baffle is further arranged on the surface of the web plate facing the heat exchange pipe, and the baffle enables the web plate to be turned over and opened under the action of fluid in the heat exchange pipe; when the catalyst is used, the ethylene oxide and the initiator in the kettle body are in an intermittent reaction process, so that a circulating pump on a heat exchange tube can generate a negative pressure adsorption effect on the catalyst in the catalytic cylinder in the starting process of intermittent operation, and the initiator in the loop tube still does not enter the loop tube; through the web of setting in the branch pipe, the negative pressure state that makes not flow through the starter in the heat exchange tube is not enough to open the web upset, and then keeps isolated between branch pipe and heat exchange tube to under the flow effect of starter, open the web upset from the branch pipe through the separation blade, and the pipe diameter that the branch pipe is less than the heat exchange tube has avoided the hindrance of the web to fluid in the heat exchange tube, thereby has promoted the preparation effect of water-reducing agent for the concrete.
The invention has the following beneficial effects:
1. the invention discharges the heat generated by the addition reaction of the initiator and the ethylene oxide in time by the arranged heat exchanger and the pipeline arranged on the kettle body, and utilizes the ejection cylinder at the top of the kettle body to react the initiator and the ethylene oxide in the gas guide tube, adjusts the initial amount in the loop pipe by the circulating pump, adjusts the reaction amount of the ethylene oxide, and then adjusts the circulating pump by the controller to achieve the control of the synthetic state of the polyether macromonomer.
2. The opening of the guide cylinder in the kettle body limits the amount of ethylene oxide entering the kettle body from the air guide pipe, so that the safety of the preparation process is enhanced; the arc-shaped bulge arranged in the spraying cylinder enables fluid in the spraying cylinder to generate a Venturi effect, and then the flow regulation range of the circulating pump in the spraying cylinder is enlarged; the blade arranged between the injection cylinder and the guide cylinder enhances the amount of ethylene oxide entering the kettle body from the air duct and maintains the stability of the supply of the ethylene oxide in the air duct.
3. According to the invention, through the web arranged in the branch pipe, the web is not enough to be opened in a turnover manner in a negative pressure state that the initiator does not flow through the heat exchange pipe, so that the isolation between the branch pipe and the heat exchange pipe is kept, the web is opened in a turnover manner from the branch pipe through the baffle plate under the flowing action of the initiator, and the obstruction of the web to fluid in the heat exchange pipe is avoided because the branch pipe is smaller than the pipe diameter of the heat exchange pipe.
Drawings
The invention is further described with reference to the following figures and embodiments.
FIG. 1 is a flow chart of a process for preparing a water reducing agent for concrete according to the present invention;
FIG. 2 is a perspective view of a loop reactor of the present invention;
FIG. 3 is a perspective view of the kettle body components of the present invention;
FIG. 4 is a cross-sectional view of a jet cartridge assembly of the present invention;
FIG. 5 is an enlarged view of a portion of FIG. 3 at A;
FIG. 6 is a partial enlarged view at B in FIG. 3;
FIG. 7 is an enlarged view of a portion of FIG. 4 at C;
in the figure: the device comprises a kettle body 1, an injection barrel 2, an arc-shaped bulge 21, an impeller 22, blades 23, a loop pipe 3, a heat exchange pipe 4, a circulating pump 41, an air guide pipe 5, a guide barrel 6, a spring 61, an opening 62, a catalytic barrel 7, a branch pipe 71, a web 72 and a baffle 721.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
As shown in FIGS. 1 to 7, the preparation process of the water reducer for concrete provided by the invention comprises the following steps:
s1, clean purging: purging nitrogen into a loop reactor for preparing the polyether macromonomer through a gas cylinder to ensure that air in a pipeline is exhausted and filled with the nitrogen, and starting an electric blanket on the outer wall of the kettle body 1 to keep the temperature of the electric blanket at 15-25 ℃;
s2, feeding and mixing: after the cleaning treatment of the loop reactor in the S1 is finished, the ethylene oxide in the storage bin is communicated with the kettle body 1 of the loop reactor through the air duct 5, the initiator pre-filled at the bottom of the kettle body 1 is pumped out through the loop pipe 3, the temperature is controlled at 24-32 ℃ through the external heat exchange pipe 4, then the initiator is led into the injection cylinder 2 of the loop reactor, the initiator is led into the kettle body 1 through the injection cylinder 2 at the top of the kettle body 1 and is mixed with the ethylene oxide input by the air duct 5, wherein the initiator is ethylene glycol containing active hydrogen;
s3, curing in a kettle: in the reaction process of the S2 kettle body 1, the circulating initiator carries the catalyst filled in the initiator into the kettle body 1 when passing through the heat exchange tube 4, the initiator and ethylene oxide are subjected to addition polymerization reaction to generate a polyether macromonomer, and the mixed liquid phase in the kettle body 1 is circulated through the heat exchange tube 4 by utilizing the loop tube 3 to ensure the full reaction between the initiator and the added ethylene oxide;
s4, finished product discharge: after the reaction is carried out in the kettle body 1 in the S3 for 120min, controlling the state of an initiator in the kettle body 1 in the reaction process to be in 10-15min intermittent operation, finally introducing nitrogen to purge residual ethylene oxide in a loop reactor pipeline, and discharging a polyether macromonomer prepared in the kettle body 1 from the bottom to be used as a raw material carrier of the polycarboxylic acid water reducing agent;
wherein, the loop reactor described in S1-S4 comprises a kettle body 1 and a controller; the top of the kettle body 1 is provided with an injection cylinder 2, and the injection cylinder 2 is communicated with the bottom of the kettle body 1 through a loop pipe 3; the loop pipe 3 is also internally provided with a heat exchange pipe 4, and the heat exchange pipe 4 is used for conducting heat of fluid inside the loop pipe; a circulating pump 41 is also arranged on a pipeline at the top of the heat exchange pipe 4, and the circulating pump 41 pumps and circulates the fluid in the kettle body 1 through the pipeline; the outer wall of the kettle body 1 is also wrapped with an electric blanket, the top of the kettle body 1 is provided with an annular opening, and the bottom of the kettle body 1 is also provided with a discharge opening; the annular opening of the kettle body 1 is positioned in the circumferential direction of the injection cylinder 2 and is provided with a communicated air duct 5, the tail end of the air duct 5 is provided with a stock bin and an air bottle which are connected in parallel, and ethylene oxide and nitrogen are respectively stored in the stock bin and the air bottle; an electromagnetic valve for controlling on-off is installed on a pipeline of the kettle body 1, and the electromagnetic valve and the circulating pump 41 operate under the regulation of the controller;
in the prior art, a polyether macromonomer raw material carrier is adopted in production of a polycarboxylate superplasticizer, the production process belongs to intermittent strong exothermic reaction, the product has high viscosity, and is easy to block reaction equipment, meanwhile, the reaction process of the combustible, explosive and highly toxic ethylene oxide gas in the reaction raw materials needs to be precisely controlled, so that potential safety hazards are avoided, and the preparation efficiency is limited;
therefore, the invention makes the added reacted ethylene oxide and the initiator react in the kettle body 1 through the pipeline arranged in the loop reactor, the heat in the reaction process is discharged in time through the heat exchange pipe 4 arranged in the loop pipe 3 and the jet cylinder 2 between the gas guide pipe 5 and the loop pipe 3, the electric blanket on the outer wall of the kettle body 1 is used for reducing the heat fluctuation range in the reaction process, and the gas guide pipe 5 reduces the content of the free ethylene oxide in the kettle body 1 in the reaction process after being blown with nitrogen for purging, simultaneously the catalyst in the heat exchanger is mixed by the initiator driven by the circulating pump 41, and then the mixture is converted into high-speed fluid through the jet cylinder 2 to be carried out in the kettle body 1, and the local negative pressure is generated in the top area of the kettle body 1 to carry out the ethylene oxide gas in the gas guide pipe 5, so that the reaction quantity of the ethylene oxide matches the initial dosage of the mixed catalyst, further controlling the synthesis of the polyether macromonomer, and taking out the prepared polyether macromonomer through a discharge port; the invention utilizes the arranged heat exchanger to match with a pipeline arranged on the kettle body 1, the heat generated by the addition reaction of the initiator and the ethylene oxide is discharged in time, the initiator reacts with the ethylene oxide in the gas guide tube 5 by utilizing the ejection tube 2 at the top of the kettle body 1, the initial amount in the loop tube 3 is adjusted by the circulating pump 41 and then fed back to the flow change in the ejection tube 2, so that the negative pressure value of the gas guide tube 5 at the top of the kettle body 1 is changed, the reaction amount of the ethylene oxide is adjusted accordingly, and the control on the synthetic state of the polyether macromonomer is achieved by adjusting the circulating pump 41 by the controller, thereby improving the preparation effect of the water reducing agent for concrete.
As an embodiment of the invention, a guide cylinder 6 is arranged between the kettle body 1 and the air duct 5, and the guide cylinder 6 communicates the annular opening of the kettle body 1 with the air duct 5; the guide cylinder 6 is sleeved and mounted at the top of the kettle body 1, a spring 61 is further mounted between the circumferential outer side of the guide cylinder 6 and the kettle body 1, and an opening 62 is formed in the inner wall of the guide cylinder 6 in the kettle body 1; the guide cylinder 6 changes the sectional area between the opening 62 and the injection cylinder 2 under the change of the negative pressure generated by the spring 61 and the injection cylinder 2, and adjusts the flow of ethylene oxide in the air duct 5; when the device is used, the controller adjusts the running state of the circulating pump 41, and further controls the negative pressure value generated by the injection cylinder 2 in the top area of the kettle body 1 to change the reaction rate between the initiator and the ethylene oxide in the kettle body 1; the kettle body 1 and the gas guide pipe 5 are communicated through the arranged guide cylinder 6, the opening 62 of the guide cylinder 6 in the kettle body 1 is utilized to enable the injection cylinder 2 to generate a negative pressure effect in a smaller fluid state, the negative pressure effect is further weakened by the spring 61 between the guide cylinder 6 and the kettle body 1, the sectional area of the opening 62 in the kettle body 1 is reduced, the amount of ethylene oxide entering the kettle body 1 through the gas guide pipe 5 is limited, the free ethylene oxide which is not reacted with an initiator is not generated in the kettle body 1, the safety of the preparation process is further enhanced, the displacement inertia generated by the guide cylinder 6 in the negative pressure increment state of the top of the kettle body 1 is reduced under the condition that the flow of the initiator is gradually increased in the injection cylinder 2, the buffer effect of the spring 61 on the guide cylinder 6 is utilized to control the stability of the reaction process in the kettle body 1, and therefore the preparation effect of the water reducing agent for concrete is improved.
As an embodiment of the present invention, an arc protrusion 21 is further disposed inside the spray cylinder 2, and the arc protrusion 21 makes the pipe diameter of the spray cylinder 2 be a symmetrical hyperboloid body; the injection cylinder 2 is rotatably arranged on the kettle body 1, and the inner wall of the bottom port of the injection cylinder 2 is also provided with an impeller 22 surrounding the bulge; when the device is used, the circulating pump 41 drives fluid to enter the injection cylinder 2 through the loop pipe 3, the impulse of the fluid is lost in the loop pipe 3, and the circulating pump 41 is required to have larger output in order to meet different reaction rates of the injection cylinder 2 on the initiator and the ethylene oxide; through setting up at the inside arc arch 21 of a section of thick bamboo 2 that sprays for fluid is when getting into the cauldron body 1 through a section of thick bamboo 2 that sprays, successively through the effect of the pipe diameter that diminishes earlier in a section of thick bamboo 2 and increase again, has played the venturi effect to the fluid in a section of thick bamboo 2 that sprays, has increased the velocity of flow of fluid in cauldron body 1 end a section of thick bamboo 2 that sprays, has increased the flow control scope of circulating pump 41 in to a section of thick bamboo 2 then, thereby has promoted the preparation effect of water-reducing agent for the concrete.
As an embodiment of the present invention, the outer wall of the injection cylinder 2 is further provided with a fixed vane 23, and the edge of the vane 23 is located in the gap between the injection cylinder 2 and the guide cylinder 6; the blades 23 rotate along with the injection cylinder 2 under the action of the impeller 22, so that the negative pressure effect on the opening 62 of the guide cylinder 6 is increased; when the device is used, ethylene oxide in the storage bin enters the kettle body 1 through the air duct 5, and the amount of the ethylene oxide entering the kettle body 1 can be weakened due to the pipeline of the air duct 5; through the blades 23 arranged between the injection cylinder 2 and the guide cylinder 6, the negative pressure value of the fluid in the injection cylinder 2 in the area of the guide cylinder 6 is further enhanced under the increment state, the ethylene oxide amount entering the kettle body 1 from the air duct 5 is enhanced, the flow of the initiator in the injection cylinder 2 is met, the reaction rate required by polyether macromonomer preparation is achieved, the ethylene oxide supply stability in the air duct 5 is maintained, and the preparation effect of the water reducing agent for concrete is improved.
As an embodiment of the invention, the heat exchange tube 4 is further provided with a catalytic cylinder 7, the catalytic cylinder 7 is communicated to the heat exchange tube 4 through a branch tube 71, and the catalytic cylinder 7 is filled with a catalyst; the branch pipe 71 is positioned at the bottom of the catalytic cylinder 7 and the heat exchange pipe 4; when the catalyst is used, the catalyst pre-installed in the heat exchange tube 4 enters the kettle body 1 along with the circulating initiator to catalyze the addition reaction between the ethylene oxide and the initiator, and in order to control the speed of the reaction process, the amount of the catalyst entering the kettle body 1 is matched with the circulation amount of the initiator in the heat exchange tube 4 as required; the catalyst is independently filled in the catalyst cylinder 7 and is arranged on the heat exchange tube 4, the heat generated in the reaction of the initiator and ethylene oxide emitted from the heat exchange tube 4 is utilized to maintain the active state temperature of the catalyst in the catalyst cylinder 7, and the branch tube 71 is positioned at the bottom positions of the catalyst cylinder 7 and the heat exchange tube 4, so that the catalyst in the catalyst cylinder 7 is accumulated to the position of the branch tube 71 on the heat exchange tube 4 under the action of gravity, the flow change of the flowing initiator entering the heat exchange tube 4 drives the amount of the catalyst stripped in the branch tube 71, and the preparation effect of the water reducing agent for concrete is improved.
As an embodiment of the present invention, the branch pipe 71 is smaller than the pipe diameter of the heat exchange pipe 4, and a rotating web 72 is further provided in the branch pipe 71; the web 72 makes the branch pipe 71 in a closed state at the port of the heat exchange pipe 4 under the action of gravity, the web 72 is further provided with a baffle 721 on the surface facing the heat exchange pipe 4, and the baffle 721 makes the web 72 turn open under the action of fluid in the heat exchange pipe 4; when the reactor is used, the ethylene oxide and the initiator in the kettle body 1 are in an intermittent reaction process, so that a circulating pump 41 on the heat exchange tube 4 can generate a negative pressure adsorption effect on the catalyst in the catalytic cylinder 7 in the starting process of intermittent operation, and the initiator in the loop tube 3 does not enter the loop tube at the moment; through the web 72 arranged in the branch pipe 71, the negative pressure state of the initiator which does not flow through the heat exchange pipe 4 is not enough to turn and open the web 72, so that the isolation between the branch pipe 71 and the heat exchange pipe 4 is kept, the web 72 is turned and opened from the branch pipe 71 through the baffle 721 under the flowing action of the initiator, and the branch pipe 71 is smaller than the pipe diameter of the heat exchange pipe 4, so that the obstruction of the web 72 to the fluid in the heat exchange pipe 4 is avoided, and the preparation effect of the water reducing agent for concrete is improved.
When in use, the ethylene oxide and the initiator are added for reaction through a pipeline arranged in the loop reactor, the mixed reaction is carried out in the kettle body 1 through the injection cylinder 2 between the gas guide pipe 5 and the loop pipe 3, the heat exchange pipe 4 arranged in the loop pipe 3 discharges the heat in the reaction process in time, the electric blanket on the outer wall of the kettle body 1 is used for reducing the heat fluctuation range in the reaction process, the gas guide pipe 5 reduces the content of the free ethylene oxide in the kettle body 1 in the reaction process after being blown with nitrogen for purging, simultaneously the catalyst in the heat exchanger is mixed by the initiator driven by the circulating pump 41, and then the mixture is converted into high-speed fluid through the injection cylinder 2 to be carried out in the kettle body 1, and local negative pressure is generated in the top area of the kettle body 1 to carry out the ethylene oxide gas in the gas guide pipe 5, so that the reaction quantity of the ethylene oxide is matched with the initial dosage of the mixed catalyst, further controlling the synthesis of the polyether macromonomer, and taking out the prepared polyether macromonomer through a discharge port; the guide tube 6 is arranged to be communicated between the kettle body 1 and the gas guide tube 5, the opening 62 of the guide tube 6 in the kettle body 1 is utilized to enable the injection tube 2 to generate a negative pressure effect in a smaller fluid state, the negative pressure effect is further weakened by the spring 61 between the guide tube 6 and the kettle body 1, the sectional area of the opening 62 in the kettle body 1 is reduced, the amount of ethylene oxide entering the kettle body 1 from the gas guide tube 5 is limited, the free ethylene oxide which is not reacted with an initiator is not generated in the kettle body 1, the safety of the preparation process of the free ethylene oxide is further enhanced, the displacement inertia generated by the guide tube 6 in a negative pressure increment state at the top of the kettle body 1 is reduced under the condition that the flow of the initiator is gradually increased in the injection tube 2, and the stability of the reaction process in the kettle body 1 is controlled by the buffer effect of the spring 61 on the guide tube 6; the arc-shaped protrusions 21 are arranged in the ejection cylinders 2, so that when fluid enters the kettle body 1 through the ejection cylinders 2, the fluid passes through the action of the pipe diameters of the ejection cylinders 2, which are reduced and increased, a Venturi effect is achieved on the fluid in the ejection cylinders 2, the flow velocity of the fluid in the ejection cylinders 2 at the ends of the kettle body 1 is increased, and then the flow regulation range of the circulating pump 41 in the ejection cylinders 2 is increased; the blades 23 arranged between the injection cylinder 2 and the guide cylinder 6 further enhance the negative pressure value of the fluid in the injection cylinder 2 in the area of the guide cylinder 6 under the increment state, enhance the amount of ethylene oxide entering the kettle body 1 from the gas guide pipe 5, meet the flow of the initiator in the injection cylinder 2, achieve the reaction rate required by the preparation of the polyether macromonomer, and maintain the stability of the supply of the ethylene oxide in the gas guide pipe 5; the catalyst cartridge 7 is arranged to be independently filled with a catalyst and is arranged on the heat exchange tube 4, the temperature of the catalyst in the catalyst cartridge 7 in an active state is maintained by utilizing the heat generated in the reaction of an initiator and ethylene oxide emitted from the heat exchange tube 4, and the branch tube 71 is positioned at the bottom positions of the catalyst cartridge 7 and the heat exchange tube 4, so that the catalyst in the catalyst cartridge 7 is accumulated to the position of the branch tube 71 on the heat exchange tube 4 under the action of gravity, and the flow change of the flowing initiator entering the heat exchange tube 4 drives the amount of the catalyst peeled off from the branch tube 71; the web 72 is arranged in the branch pipe 71, so that the negative pressure state of the heat exchange pipe 4 without flowing the initiator is not enough to open the web 72 in a turnover way, the isolation between the branch pipe 71 and the heat exchange pipe 4 is further kept, the web 72 is opened in a turnover way from the branch pipe 71 through the baffle 721 under the flowing action of the initiator, and the branch pipe 71 is smaller than the pipe diameter of the heat exchange pipe 4, so that the web 72 avoids the obstruction of the fluid in the heat exchange pipe 4.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A preparation process of a water reducing agent for concrete is characterized by comprising the following steps:
s1, clean purging: purging nitrogen into a loop reactor for preparing the polyether macromonomer through a gas cylinder to ensure that air in a pipeline is exhausted and filled with the nitrogen, and starting an electric blanket on the outer wall of the kettle body (1) to maintain the temperature of the kettle body at 15-25 ℃;
s2, feeding and mixing: after the cleaning treatment of the loop reactor in S1 is completed, the ethylene oxide in the storage bin is communicated with the kettle body (1) of the loop reactor through the air duct (5), the initiator pre-filled at the bottom of the kettle body (1) is pumped out through the loop pipe (3), the temperature is controlled to be 24-32 ℃ through the external heat exchange pipe (4), then the temperature is controlled to be in the range of 24-32 ℃ and the initiator is led into the kettle body (1) through the injection cylinder (2) at the top of the kettle body (1) and mixed with the ethylene oxide input by the air duct (5), wherein the initiator is ethylene glycol containing active hydrogen;
s3, curing in a kettle: in the reaction process of the S2 kettle body (1), when flowing initiator passes through the heat exchange tube (4), the catalyst filled in the initiator is brought into the kettle body (1), the initiator and ethylene oxide are subjected to addition polymerization reaction to generate polyether macromonomer, and the mixed liquid phase in the kettle body (1) is circulated through the heat exchange tube (4) by utilizing the loop tube (3), so that the initiator and the added ethylene oxide are ensured to be fully reacted;
s4, finished product discharge: after the reaction is carried out in the kettle body (1) in S3 for 120min, controlling the state of an initiator in the kettle body (1) to be extracted in the reaction process to be in 10-15min intermittent operation, finally introducing nitrogen to purge residual ethylene oxide in a loop reactor pipeline, and discharging a polyether macromonomer prepared in the kettle body (1) from the bottom to be used as a raw material carrier of the polycarboxylic acid water reducing agent;
wherein the loop reactor described in S1-S4 comprises a kettle body (1) and a controller; the top of the kettle body (1) is provided with an injection cylinder (2), and the injection cylinder (2) is communicated with the bottom of the kettle body (1) through a loop pipe (3); a heat exchange tube (4) is further arranged in the loop tube (3), and the heat exchange tube (4) is used for conducting heat of fluid inside the heat exchange tube; a circulating pump (41) is further installed on a pipeline at the top of the heat exchange pipe (4), and the circulating pump (41) enables fluid in the kettle body (1) to be pumped and circulated through the pipeline; the outer wall of the kettle body (1) is also wrapped with an electric blanket, the top of the kettle body (1) is provided with an annular opening, and the bottom of the kettle body (1) is also provided with a discharge opening; the annular opening of the kettle body (1) is positioned on the circumferential direction of the injection cylinder (2) and is provided with a communicated air duct (5), the tail end of the air duct (5) is provided with a stock bin and an air bottle which are connected in parallel, and ethylene oxide and nitrogen are respectively stored in the stock bin and the air bottle; the pipeline of the kettle body (1) is provided with an electromagnetic valve for controlling on-off, and the electromagnetic valve and the circulating pump (41) run under the regulation of the controller.
2. The preparation process of the water reducing agent for concrete according to claim 1, characterized by comprising the following steps: a guide cylinder (6) is also arranged between the kettle body (1) and the air guide pipe (5), and the guide cylinder (6) communicates the annular opening of the kettle body (1) with the air guide pipe (5); the guide cylinder (6) is sleeved and mounted at the top of the kettle body (1), a spring (61) is further mounted between the circumferential outer side of the guide cylinder (6) and the kettle body (1), and an opening (62) is formed in the inner wall of the guide cylinder (6) in the kettle body (1); the guide cylinder (6) changes the sectional area between the opening (62) and the injection cylinder (2) under the change of the negative pressure action generated by the spring (61) and the injection cylinder (2), and adjusts the flow rate of ethylene oxide in the air duct (5).
3. The preparation process of the water reducing agent for concrete according to claim 2, characterized by comprising the following steps: an arc-shaped bulge (21) is further arranged inside the injection cylinder (2), and the arc-shaped bulge (21) enables the pipe diameter of the injection cylinder (2) to be a symmetrical hyperboloid body; the spraying cylinder (2) is rotatably arranged on the kettle body (1), and a surrounding convex impeller (22) is further arranged on the inner wall of the bottom port of the spraying cylinder (2).
4. The preparation process of the water reducing agent for concrete according to claim 3, characterized by comprising the following steps: the outer wall of the injection cylinder (2) is also provided with fixed blades (23), and the edges of the blades (23) are positioned in a gap between the injection cylinder (2) and the guide cylinder (6); the blades (23) rotate along with the injection cylinder (2) under the action of the impeller (22) in the same way, so that the negative pressure effect on the opening (62) of the guide cylinder (6) is increased.
5. The preparation process of the water reducing agent for concrete according to claim 1, characterized by comprising the following steps: the heat exchange tube (4) is also provided with a catalytic cylinder (7), the catalytic cylinder (7) is communicated to the heat exchange tube (4) through a branch tube (71), and a catalyst is filled in the catalytic cylinder (7); the branch pipe (71) is positioned at the bottom of the catalytic cylinder (7) and the heat exchange pipe (4).
6. The preparation process of the water reducing agent for concrete according to claim 5, characterized by comprising the following steps: the branch pipe (71) is smaller than the pipe diameter of the heat exchange pipe (4), and a rotary web plate (72) is further arranged in the branch pipe (71); the web (72) enables the branch pipe (71) to be in a closed state at the port of the heat exchange pipe (4) under the action of gravity, a baffle plate (721) is further arranged on the surface, facing the heat exchange pipe (4), of the web (72), and the web (72) is turned over and opened under the action of fluid in the heat exchange pipe (4) through the baffle plate (721).
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Cited By (1)
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