CN109517100B - Chlorinated polyvinyl chloride resin and preparation method thereof - Google Patents

Chlorinated polyvinyl chloride resin and preparation method thereof Download PDF

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CN109517100B
CN109517100B CN201811253357.5A CN201811253357A CN109517100B CN 109517100 B CN109517100 B CN 109517100B CN 201811253357 A CN201811253357 A CN 201811253357A CN 109517100 B CN109517100 B CN 109517100B
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chlorine
chlorination
polyvinyl chloride
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chlorinated polyvinyl
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CN109517100A (en
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金胜波
王曙光
韩风
凌玉英
胡海波
侯兰明
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Shandong Gaoxin Chemical Co ltd
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Abstract

The invention discloses a chlorinated polyvinyl chloride resin and a preparation method thereof, and the chlorinated polyvinyl chloride resin comprises the following steps: the preparation method comprises the steps of preparation of a suspension solution, PVC resin infiltration, chlorination, deacidification, neutralization, centrifugation and drying; the chlorination process step is an oxygen-free atmosphere; the chlorination process step is to introduce chlorine according to a chlorination program; the chlorine gas is introduced into the bottom of the chlorination kettle in a liquid chlorine introducing mode. The chlorine content of the obtained chlorinated polyvinyl chloride resin reaches 66-72%, the tensile strength is more than or equal to 50MPa, the Vicat softening temperature is more than or equal to 120 ℃, and the dynamic thermal stability time is more than or equal to 25 min. Compared with the prior art, the Vicat softening temperature is increased by 5-10 ℃, the dynamic heat resistance is increased by 5-15min, and the comprehensive performance is excellent; the reaction time is shortened, the production efficiency is improved by 25 to 50 percent, and the service life of equipment is prolonged by 50 to 200 percent; hydrochloric acid and condensed water required for preparing the suspension solution come from a chlorination process and a drying process, so that the cyclic utilization of the hydrochloric acid solution is realized, the heat value of the condensed water is effectively utilized, the comprehensive utilization of heat and water resources is realized, and the energy-saving and environment-friendly effects are realized.

Description

Chlorinated polyvinyl chloride resin and preparation method thereof
Technical Field
The invention relates to chlorinated polyvinyl chloride resin and a preparation method thereof, belonging to the technical field of chemical industry.
Background
In recent years, with technological progress, new materials have been developed in various fields of China. Chlorinated polyvinyl chloride has a wide prospect as a new material. Besides the excellent properties of polyvinyl chloride, the polyvinyl chloride has the characteristics of stronger corrosion resistance, heat resistance, flame retardance, higher mechanical strength, good electrical properties and the like. Can replace some traditional thermoplastic engineering plastics in a certain range, and has excellent cost performance. The method is widely applied to the fields of chemical industry, building materials, electric appliances, adhesives and the like.
The CPVC is produced by an aqueous phase suspension method, which is a commonly adopted production method at present. The method takes water or hydrochloric acid as a medium, and the chlorinated polyvinyl chloride is obtained by chemical reaction under the combined action of temperature, pressure and initiation process. The production process is heterogeneous reaction, and how to improve the uniformity of chlorination, feasible reaction conditions and excellent product performance is a technical problem to be solved in the field.
The prior published aqueous phase suspension chlorination method has different processes of different manufacturers, for example, patent application No. CN021354721 discloses an aqueous phase suspension ultraviolet light preparation method of chlorinated polyvinyl chloride, which adopts ultraviolet light irradiation, the reaction pressure is 0.2-0.4MPa, the temperature is 70-100 ℃, the reaction time is 4h-6h, and CPVC resin with the chlorine content of 61-68%, the thermal decomposition temperature is 110 ℃, and the thermal stability time is more than 60 seconds is obtained. The invention solves the problem of no decomposition during long-term storage, but has low chlorine content and poor heat resistance.
Patent application No. CN201310231633.9 discloses a chlorinated polyvinyl chloride resin, a preparation method and application thereof, which comprises the following steps: (1) in an oxygen-free atmosphere, introducing chlorine into a mixed system of the polyvinyl chloride resin, the initiator, the dispersant and water or hydrochloric acid, and adjusting the chlorine introducing speed and the chlorine introducing time to obtain a mixture with the chlorine content of 63-66% and the Vicat softening temperature of 95-105 ℃. The chlorinated polyvinyl chloride resin prepared by the method has low chlorine content and poor thermal stability.
Patent application No. CN2009101166283 discloses a method for producing chlorinated polyvinyl chloride resin with high chlorine content by one-step method, which increases the pressure in a kettle to 0.5-0.6MPa, increases the solubility of chlorine in water to improve the uniformity of chlorine and the chlorine content. The reaction time is 5-6h, and the chlorine content of the obtained product is 70%. The invention relates to a product with high chlorine content, but high pressure in the reaction process and strict requirements on equipment.
In summary, the chlorination method by aqueous phase suspension method in the prior art has the following problems: the prepared chlorinated polyvinyl chloride resin has poor chlorination uniformity; insufficient thermal stability; the chlorination condition is harsh, the reaction time is long, and the production efficiency of the product is low; the product has low comprehensive performance.
Disclosure of Invention
The invention aims to solve the technical problems and provides chlorinated polyvinyl chloride resin and a production method thereof so as to realize the following purposes: the chlorination uniformity of the chlorinated polyvinyl chloride resin is improved; the thermal stability of the chlorinated polyvinyl chloride resin is improved; the chlorination reaction time is shortened, and the production efficiency of products is improved; the comprehensive performance of the product is improved; the hydrochloric acid generated by the chlorination reaction is recycled, so that the energy is saved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of chlorinated polyvinyl chloride resin comprises the following steps: the preparation method comprises the steps of preparation of a suspension solution, PVC resin infiltration, chlorination, deacidification, neutralization, centrifugation and drying; the chlorination process step is carried out in an oxygen-free atmosphere.
The preparation of the suspension solution and the PVC resin infiltration step are that 1000 parts of prepared hydrochloric acid solution, 100 parts of PVC resin, 280 parts of dispersant, 0.35-3.5 parts of anti-sticking agent and 0.2-2.0 parts of initiator are added into a batching tank by weight part, and stirred to prepare the suspension solution which is heated and infiltrated.
The infiltration mode is that the hydrochloric acid solution is heated and infiltrated, the suspension solution is evenly heated from room temperature to the infiltration temperature and then infiltrated for 10min to 60min, the infiltration temperature is 50 ℃ to 80 ℃, and the heating time is 15min to 40 min.
The concentration of the hydrochloric acid solution is 0-21%.
And the chlorination process step comprises introducing liquid chlorine according to a chlorination program.
The chlorination process comprises the following steps that in the chlorination procedure, the initial temperature T0 is 50-80 ℃, the final temperature T3 is 80-130 ℃, the intermediate temperature T1= T0+ (T3-T0) x (40% -60%), and the intermediate temperature T2 = T0+ (T3-T0) x (60% -80%).
The total chlorine passing amount is the chlorine passing amount required by the chlorinated polyvinyl chloride product with the chlorine content reaching 66-72%, and the corresponding chlorine passing amount in the chlorine passing program T0-T1 interval is 25-40% of the total chlorine passing amount; the corresponding chlorine passing amount in the interval of T1-T2 is 35% -55% of the total chlorine passing amount; the corresponding chlorine passing amount in the interval of T2-T3 is 5% -40% of the total chlorine passing amount.
The ratio of the total chlorine flux to the PVC resin is 1: 0.9-1.8.
The chlorine introducing time corresponding to the interval between the chlorination programs T0 and T1 is 1h-1.5 h; the corresponding chlorine introducing time in the interval of T1-T2 is 1.0h-1.8 h; the corresponding chlorine introducing time in the interval of T2-T3 is 0.3-0.8 h.
And in the chlorination process step, the chlorine gas is introduced in a mode that liquid chlorine is introduced into the bottom of the chlorination kettle.
And in the bottom chlorine introducing mode, liquid chlorine conveyed from the outside enters an inlet of a bottom valve of the chlorination kettle along a liquid chlorine guide pipe after being metered by a chlorine mass flow meter, a chlorine automatic valve and a manual valve, and enters PVC suspension solution through a chlorine distributor connected with the tail end of the guide pipe to react.
The pressure of the introduced liquid chlorine is 1.0-1.5MPa, and the depth of the chlorine distributor immersed in the suspension is 20-60 cm.
The chlorine automatic valve adopts pneumatic and electric forms.
The manual valve is a stop valve or a ball valve
The chlorination process comprises the steps that the reaction temperature is 50-130 ℃, and the pressure in a kettle in the reaction process is less than or equal to 0.50 MPa. The reaction time is 2.5-4.5h, chlorine introduction is finished, and the temperature is kept for 10-40 min.
The oxygen-free atmosphere is formed by one or a combination of a plurality of modes of vacuumizing, blowing inert gas and blowing a small amount of chlorine.
The polymerization degree of the PVC resin is 450-1500, the average particle size is 100-300 mu m, and the apparent density is more than or equal to 0.45 g/ml.
The dispersing agent is one or two of sodium dodecyl benzene sulfonate, sodium methacrylate, a copolymer of ethylene oxide and propylene oxide, polyvinylpyrrolidone and polyether surfactant;
the anti-sticking agent is one of talcum powder and silicon dioxide;
the initiator is one or two of Benzoyl Peroxide (BPO), Azobisisobutyronitrile (AIBN), Azobisisoheptonitrile (ABVN), hydrogen peroxide and cumyl peroxide (DCP).
And deacidifying, neutralizing, centrifugally dewatering and drying the chlorinated polyvinyl chloride slurry to obtain the chlorinated polyvinyl chloride resin.
And in the neutralization step, conveying the deacidified chlorinated polyvinyl chloride material to a neutralization kettle, adding tap water or deionized water in a ratio of 1:3-5, heating to a set temperature under a stirring state, and keeping the temperature for 1-8 h at the set temperature. When the temperature of the solution is 40-60 ℃, the neutralizer is uniformly added, the pH value of the solution is continuously tested, and the testing frequency is 1 time/20 min. The end point of neutralization is reached when the pH of the solution is 7-8.
The temperature of the neutralization step is set to be 75-95 ℃, and the heating rate is 3 ℃/10min-10 ℃/10 min.
The neutralizing agent comprises one or two of sodium carbonate, sodium hydroxide, sodium citrate and sodium metasilicate.
The chlorinated polyvinyl chloride resin has chlorine content of 66-72%, tensile strength not lower than 50MPa, Vicat softening temperature not lower than 120 deg.c and dynamic heat stability time not lower than 25 min.
After the technical scheme is adopted, the invention has the following beneficial effects:
1. the chlorine content of the obtained chlorinated polyvinyl chloride resin reaches 66-72%, the tensile strength is more than or equal to 50MPa, the Vicat softening temperature is more than or equal to 120 ℃, and the dynamic thermal stability time is more than or equal to 25 min. Compared with the prior art, the Vicat softening temperature is increased by 5-10 ℃, the dynamic heat resistance is increased by 5-15min, and the comprehensive performance is excellent.
2. By the soaking of the PVC resin and the program control of the chlorination process, the uniformity of chlorination is improved, the reaction time is shortened, and the comprehensive performance of the product is improved.
3. The bottom is filled with chlorine for implementation, the chlorination reaction efficiency is improved, the reaction time is shortened, and the production efficiency is improved by 25-50%. The service life of the equipment can be prolonged by 50-200%.
4. Hydrochloric acid and condensed water required for preparing the suspension solution come from a chlorination process and a drying process, wherein the hydrochloric acid comes from hydrochloric acid generated in the chlorination process, and the condensed water comes from the condensed water generated in the drying process, so that the cyclic utilization of the hydrochloric acid solution is realized, the heat value of the condensed water is effectively utilized, the comprehensive utilization of heat and water resources is realized, and the energy-saving and environment-friendly effects are realized.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1
Chlorinated polyvinyl chloride resin and a production method thereof, comprising the following steps: preparation of suspension solution, soaking in PVC resin, chlorination, deacidification, neutralization, centrifugal dehydration, and drying
(1) Preparation of suspension solution and impregnation with PVC resin
In a batching tank, hydrochloric acid solution with the concentration of 3 percent (weight ratio) is prepared by hydrochloric acid and condensed water, and the concentration is 4m3Adding 1050kg of PVC resin, 10kg of sodium methacrylate and 1.2kg of benzoyl peroxide, stirring to prepare a suspension solution, heating to 80 ℃, and soaking for 30 min.
The PVC resin is chlorinated special polyvinyl chloride, the polymerization degree is 1000, the average particle size is 200 mu m, and the apparent density is 0.50 g/ml.
(2) Chlorination of
And (3) pressing the suspension solution into a chlorination kettle, introducing nitrogen with the pressure of 0.1MPa for 30min, and removing oxygen in the chlorination kettle.
During the chlorination, the initial reaction temperature T0 was 75 ℃, the temperature T1 was 105 ℃, the temperature T2 was 108 ℃ and the final reaction temperature T3 was 128 ℃. The total chlorine flux was 1086kg, the chlorine flux in the interval T0-T1 was 326kg, the chlorine passage time was 1.2h, the chlorine flux in the interval T1-T2 was 591kg, the chlorine passage time was 1.3h, the chlorine flux in the interval T2-T3 was 169kg, and the chlorine passage time was 0.9 h. And (5) after chlorine introduction, keeping the temperature for 20 min. The reaction pressure is less than or equal to 0.45 MPa.
After being measured by a chlorine mass flow meter, an automatic chlorine valve and a manual valve, liquid chlorine conveyed from the outside enters an inlet of a bottom valve of the chlorination kettle along a liquid chlorine guide pipe, and enters PVC suspension solution through a chlorine distributor connected with the tail end of the guide pipe to participate in chlorination reaction. The pressure of the introduced liquid chlorine is 1.0MPa, and the depth of the chlorine distributor immersed in the suspension is 20 cm.
(3) Deacidifying, neutralizing, centrifuging, and drying
And deacidifying, neutralizing, centrifugally dewatering and drying the chlorinated polyvinyl chloride slurry to obtain the chlorinated polyvinyl chloride resin.
Wherein the neutralization step is as follows: conveying the deacidified chlorinated polyvinyl chloride material to a neutralization kettle, adding tap water, heating to 90 ℃ at a heating rate of 8 ℃/10min under a stirring state, and keeping the temperature at 90 ℃ for 2h, wherein the ratio of the material to the water is 1: 4. When the temperature of the solution is 50 ℃, sodium carbonate is added uniformly, the pH value of the solution is tested continuously, and the testing frequency is 1 time/20 min. The end point of neutralization was reached when the solution had a pH of 8.
The hydrochloric acid separated in the deacidification process enters a hydrochloric acid storage tank and is used for preparing a hydrochloric acid solution or selling.
And (4) the condensed water generated in the drying process enters a condensed water storage tank and is used for preparing a hydrochloric acid solution or supplementing process water.
(4) Results
The prepared chlorinated polyvinyl chloride resin has the chlorine content of 71.6 percent, the tensile strength of 62MPa, the Vicat softening temperature of 131 ℃ and the dynamic thermal stabilization time of 28 min.
Example 2
Chlorinated polyvinyl chloride resin and a production method thereof, comprising the following steps: preparation of suspension solution, soaking in PVC resin, chlorination, deacidification, neutralization, centrifugal dehydration, and drying
(1) Preparation of suspension solution and impregnation with PVC resin
In a batching tank, hydrochloric acid solution with the concentration of 15 percent (weight ratio) is prepared by hydrochloric acid and condensed water, and the concentration is 20m3Adding 3000kg of PVC resin, 15kg of copolymer of ethylene oxide and propylene oxide, 5kg of polyvinylpyrrolidone, 2.8kg of benzoyl peroxide, 1.2kg of hydrogen peroxide and 40kg of talcum powder, stirring to prepare a suspension solution, heating to 50 ℃, and infiltrating for 10 min.
The PVC resin is chlorinated special polyvinyl chloride, the polymerization degree is 1300, the average particle size is 250 mu m, and the apparent density is 0.45 g/ml.
(2) Chlorination of
Pressing the suspension solution into a chlorination kettle, sealing, introducing nitrogen with the pressure of 0.1MPa for 30min, vacuumizing to-0.06 MPa, and discharging oxygen in the chlorination kettle.
During the chlorination, the initial reaction temperature T0 was 60 ℃, the temperature T1 was 90 ℃, the temperature T2 was 100 ℃ and the final reaction temperature T3 was 110 ℃. Setting the total chlorine flux as 2250kg, the chlorine flux in the interval T0-T1 as 893kg, the chlorine flux time as 1.5h, the chlorine flux in the interval T1-T2 as 1238kg, the chlorine flux time as 1.0h, the chlorine flux in the interval T2-T3 as 119kg and the chlorine flux time as 0.3 h. And (5) after chlorine introduction, keeping the temperature for 10 min. The pressure in the kettle is less than or equal to 0.4MPa in the reaction process.
After being measured by a chlorine mass flow meter, an automatic chlorine valve and a manual valve, liquid chlorine conveyed from the outside enters an inlet of a bottom valve of the chlorination kettle along a liquid chlorine guide pipe, and enters PVC suspension solution through a chlorine distributor connected with the tail end of the guide pipe to participate in chlorination reaction. The pressure of the introduced liquid chlorine is 1.5MPa, and the depth of the chlorine distributor immersed in the suspension is 40 cm.
(3) Deacidifying, neutralizing, centrifuging, and drying
And deacidifying, neutralizing, centrifugally dewatering and drying the chlorinated polyvinyl chloride slurry to obtain the chlorinated polyvinyl chloride resin.
Wherein the neutralization step is as follows: conveying the deacidified chlorinated polyvinyl chloride material to a neutralization kettle, adding tap water, heating to 80 ℃ at a heating rate of 5 ℃/10min under a stirring state, and keeping the temperature at 80 ℃ for 6h, wherein the ratio of the material to the water is 1: 4. When the temperature of the solution is 50 ℃, the sodium hydroxide is added uniformly, the pH value of the solution is tested continuously, and the testing frequency is 1 time/20 min. The end point of neutralization was reached when the solution had a pH of 8.
The hydrochloric acid separated in the deacidification process enters a hydrochloric acid storage tank and is used for preparing a hydrochloric acid solution or selling.
And (4) the condensed water generated in the drying process enters a condensed water storage tank and is used for preparing a hydrochloric acid solution or supplementing process water.
(4) Results
The chlorine content of the prepared chlorinated polyvinyl chloride resin reaches 68.5 percent, the tensile strength is 57MPa, the Vicat softening temperature is 128 ℃, and the dynamic thermal stabilization time is 30 min.
Example 3
Chlorinated polyvinyl chloride resin and a production method thereof, comprising the following steps: preparation of suspension solution and PVC resin infiltration, chlorination process, deacidification, neutralization, centrifugal dehydration and drying
(1) Preparation of suspension solution and impregnation with PVC resin
In the batching tank, 4m of condensed water is added3720kg of PVC resin, 2.0kg of dispersant sodium dodecyl benzene sulfonate, 1.2kg of polyether surfactant, 3.0kg of initiator benzoyl peroxide and 1.8kg of azobisisobutyronitrile are added and stirred to prepare a suspension solution, the temperature is raised to 75 ℃, and the soaking time is 40 min.
The PVC resin is chlorinated special polyvinyl chloride, the polymerization degree is 800, the average particle size is 180 mu m, and the apparent density is 0.50 g/ml.
(2) Chlorination of
And (3) pressing the suspension solution into a chlorination kettle, introducing nitrogen with the pressure of 0.1MPa for 40min, and removing oxygen in the chlorination kettle.
During the chlorination, the initial reaction temperature T0 was 75 ℃, the temperature T1 was 83.5 ℃, the temperature T2 was 89.1 ℃ and the final reaction temperature T3 was 95 ℃. The total chlorine passing amount is 440kg, the chlorine passing amount in a T0-T1 interval is 154kg, the chlorine passing time is 1.3h, the chlorine passing amount in a T1-T2 interval is 220kg, the chlorine passing time is 1.4h, the chlorine passing amount in a T2-T3 interval is 66kg, and the chlorine passing time is 1.1 h. And (5) after chlorine introduction, keeping the temperature for 30 min. The reaction pressure is less than or equal to 0.45MPa
After being measured by a chlorine mass flow meter, an automatic chlorine valve and a manual valve, liquid chlorine conveyed from the outside enters an inlet of a bottom valve of the chlorination kettle along a liquid chlorine guide pipe, and enters PVC suspension solution through a chlorine distributor connected with the tail end of the guide pipe to participate in chlorination reaction. The pressure of the introduced liquid chlorine is 1.0MPa, and the depth of the chlorine distributor immersed in the suspension is 25 cm.
(3) Deacidifying, neutralizing, centrifuging, and drying
And deacidifying, neutralizing, centrifugally dewatering and drying the chlorinated polyvinyl chloride slurry to obtain the chlorinated polyvinyl chloride resin.
Wherein the neutralization step is as follows: conveying the deacidified chlorinated polyvinyl chloride material to a neutralization kettle, adding tap water, heating to 85 ℃ at a heating rate of 3 ℃/10min under a stirring state, and keeping the temperature at 85 ℃ for 5h, wherein the ratio of the material to the water is 1: 4. When the temperature of the solution is 50 ℃, sodium carbonate is added uniformly, the pH value of the solution is tested continuously, and the testing frequency is 1 time/20 min. The end point of neutralization was reached when the solution had a pH of 8.
The hydrochloric acid separated in the deacidification process enters a hydrochloric acid storage tank and is used for preparing a hydrochloric acid solution or selling.
And (4) the condensed water generated in the drying process enters a condensed water storage tank and is used for preparing a hydrochloric acid solution or supplementing process water.
(4) Results
The chlorine content of the prepared chlorinated polyvinyl chloride resin reaches 66.5 percent, the tensile strength is 52MPa, the Vicat softening temperature is 123 ℃, and the dynamic thermal stabilization time is 26 min.
Comparative example 1
3500kg of water and 800kg of PVC resin are added into a 5000L reaction kettle, 7.5kg of sodium polymethacrylate is added, the mixture is stirred uniformly, chlorine gas is introduced from room temperature, the final reaction temperature is 95 ℃, the reaction pressure is 0.4MPa, the amount of introduced chlorine gas is 480kg, and the reaction time is 6 h. And washing, neutralizing, centrifuging and drying chlorinated polyvinyl chloride slurry obtained by the reaction to obtain the chlorinated polyvinyl chloride resin. The chlorine content was 66%, the Vicat softening temperature was 108 ℃ and the static thermal stabilization time was 65 seconds.
Unless otherwise specified, the proportions in the present invention are mass proportions, and the percentages are mass percentages.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (3)

1. A preparation method of chlorinated polyvinyl chloride resin is characterized by comprising the following steps: the method comprises the following steps: the preparation method comprises the steps of preparation of a suspension solution, PVC resin infiltration, chlorination, deacidification, neutralization, centrifugation and drying;
the infiltration mode is that the hydrochloric acid solution is heated and infiltrated, the suspension solution is evenly heated from room temperature to the infiltration temperature and then infiltrated for 10min to 60min, the infiltration temperature is 50 ℃ to 80 ℃, and the heating time is 15min to 40 min;
the concentration of the hydrochloric acid solution is 0-21%;
the chlorination process step is carried out in an oxygen-free atmosphere, and chlorine is introduced according to a chlorination procedure in a manner that liquid chlorine is introduced into the bottom of a chlorination kettle;
the bottom chlorine introducing mode is that externally conveyed liquid chlorine is metered by a chlorine mass flow meter, enters an inlet of a chlorination kettle bottom valve along a liquid chlorine guide pipe after passing through a chlorine automatic valve and a manual valve, and enters PVC suspension solution through a chlorine distributor connected with the tail end of the guide pipe to react;
the chlorination procedure: the total chlorine passing amount is the required chlorine passing amount of 66-72% of the chlorine content of the obtained chlorinated polyvinyl chloride product, and the corresponding chlorine passing amount in the interval of the chlorination program T0-T1 is 25-40% of the total chlorine passing amount; the corresponding chlorine passing amount in the interval of T1-T2 is 35% -55% of the total chlorine passing amount; the corresponding chlorine passing amount in the interval of T2-T3 is 5% -40% of the total chlorine passing amount;
the chlorine introducing time corresponding to the interval from T0 to T1 is 1h to 1.5 h; the corresponding chlorine introducing time in the interval of T1-T2 is 1.0h-1.8 h; the corresponding chlorine introducing time in the interval of T2-T3 is 0.3h-0.8 h;
the pressure of the introduced liquid chlorine is 1.0-1.5MPa, and the depth of the chlorine distributor immersed in the suspension is 20-60 cm;
the method comprises the following steps of (1) carrying out neutralization, namely conveying deacidified chlorinated polyvinyl chloride materials to a neutralization kettle, adding tap water or deionized water, wherein the ratio of the materials to the water is 1:3-5, heating to a set temperature under a stirring state, and keeping the temperature for 1-8 h at the set temperature;
uniformly adding a neutralizing agent when the temperature of the solution is 40-60 ℃, continuously testing the pH value of the solution, wherein the testing frequency is 1 time/20 min, and reaching the neutralization end point when the pH value of the solution is 7-8;
the temperature in the neutralization step is set to be 75-95 ℃, and the heating rate is 3 ℃/10min-10 ℃/10 min;
the neutralizing agent comprises one or two of sodium carbonate, sodium hydroxide, sodium citrate and sodium metasilicate;
the chlorinated polyvinyl chloride resin has chlorine content of 66-72%, tensile strength not lower than 50MPa, Vicat softening temperature not lower than 120 deg.c and dynamic heat stability time not lower than 25 min.
2. The method for preparing a chlorinated polyvinyl chloride resin according to claim 1, wherein: the preparation of the suspension solution and the PVC resin infiltration step are that 1000 parts of prepared hydrochloric acid solution, 100 parts of PVC resin, 280 parts of dispersant, 0.35-3.5 parts of anti-sticking agent and 0.2-2.0 parts of initiator are added into a batching tank by weight part, and stirred to prepare the suspension solution which is heated and infiltrated.
3. The method for preparing a chlorinated polyvinyl chloride resin according to claim 1, wherein: the chlorination procedure is initiated at a temperature T0 of 50-80 ℃, a final temperature T3 of 80-130 ℃, an intermediate temperature T1= T0+ (T3-T0) × (40% -60%), and an intermediate temperature T2 = T0+ (T3-T0) × (60% -80%).
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