CN113717515B - Antistatic heat-insulating plastic pipe and preparation method thereof - Google Patents
Antistatic heat-insulating plastic pipe and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
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- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6558—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom containing at least two different or differently substituted hetero rings neither condensed among themselves nor condensed with a common carbocyclic ring or ring system
- C07F9/65583—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom containing at least two different or differently substituted hetero rings neither condensed among themselves nor condensed with a common carbocyclic ring or ring system each of the hetero rings containing nitrogen as ring hetero atom
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/0038—Use of organic additives containing phosphorus
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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Abstract
The invention relates to an antistatic heat-insulating plastic pipe and a preparation method thereof, belonging to the technical field of heat-insulating materials, wherein the plastic pipe comprises the following raw materials: polyol mixture, foaming agent, catalyst, cross-linking agent, additive, polyisocyanate and heat insulation filler; the preparation method of the plastic pipe comprises the following steps: firstly, uniformly mixing part of raw materials to obtain a mixture; secondly, adding polyisocyanate and heat insulation filler into the mixture at the temperature of 20-35 ℃, then stirring the materials, pouring the materials into a mould for foaming and molding, and then demoulding; and thirdly, after demolding, post-curing treatment is carried out. The additive is prepared, the flame-retardant component with the flame-retardant effect and the quaternary ammonium salt structure are combined, so that the additive generates synergy, and simultaneously plays the flame-retardant and antistatic effects on the premise of not influencing the heat preservation and insulation effects of the antistatic heat-preservation plastic pipe.
Description
Technical Field
The invention belongs to the technical field of heat insulation materials, and particularly relates to an antistatic heat insulation plastic pipe and a preparation method thereof.
Background
Thermal insulation materials are used in large quantities in various industrial pipelines, kilns, buildings, etc. But is very sensitive to static electricity, and is easy to generate potential safety hazards such as fire hazard and the like under the condition of static electricity. For example, most coal mining mines are deep wells below 500 meters underground at present, the underground temperature is increased by 2-3 ℃ every 100 meters deep underground above 500 meters, and the temperature is higher in the deep wells, so that the working environment of the mining industry is worsened. In order to improve such working environment, it is necessary to improve the working environment by performing cold and hot replacement in the deep well. In the prior art, when a small amount of deep-well coal mines are exploited, an ice refrigeration method is adopted. That is, ice is first made on the well and then transported downhole to change the ambient temperature. This approach is costly, inefficient, and ineffective. The method adopted at present is to convey cold fluid medium to the deep well for recycling. Because the pipeline is used for a deep well and the temperature of a cold fluid medium is also ensured, certain requirements are required for heat preservation, safety, flame retardance and static resistance.
Disclosure of Invention
In order to overcome the technical problems mentioned in the background art, the invention aims to provide an antistatic heat-insulating plastic pipe and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
an antistatic heat-insulating plastic pipe comprises the following raw materials in parts by weight:
80 parts of polyol mixture, 20-30 parts of foaming agent, 1-3 parts of catalyst, 1-2 parts of cross-linking agent, 15-25 parts of additive, 95-100 parts of polyisocyanate and 8-12 parts of heat insulation filler;
the additive is prepared by the following steps:
mixing the flame-retardant component and isopropanol, adding sodium chloroacetate while stirring at the temperature of 80-90 ℃, adding sodium hydroxide in the reaction process to adjust the pH value to 7-9, then carrying out heat preservation reaction for 4 hours, and after the reaction is finished, carrying out reduced pressure concentration to remove the solvent to obtain the additive.
Further, the amount ratio of the flame retardant component to isopropyl alcohol was 1g:10mL; the mass ratio of the flame-retardant component to the sodium chloroacetate is 7.5:2.4.
further, the flame retardant component is prepared by the steps of:
step S11, adding lauric acid and xylene into a reaction kettle, connecting a water diversion device, adding diethylenetriamine, heating to 140 ℃ until water is separated out, then continuing heating to 240 ℃, reacting until water is not separated out, then cooling to 120 ℃, concentrating under reduced pressure, removing a solvent, then recrystallizing with acetone, and then drying at 40 ℃ to constant weight to obtain an intermediate 1; wherein the dosage ratio of lauric acid, diethylenetriamine and xylene is 0.1mol:0.1mol:30mL;
the reaction process is as follows:
s12, mixing cyanuric chloride and a solvent, then mixing sodium hydroxide and an aqueous solution of the intermediate 1, adding the mixture, controlling the speed in the adding process, keeping the temperature at 0 ℃ and the pH value at about 6, and reacting for 2 hours to obtain an intermediate 2; wherein the solvent is one of acetone, dioxane and deionized water; aqueous solution of intermediate 1 was intermediate 1 and deionized water according to 13g:20mL of the mixture is mixed; the dosage ratio of cyanuric chloride, solvent and sodium hydroxide is 0.1mol:60mL of: 0.1mmol; the molar ratio of the cyanuric chloride to the intermediate 1 is 1:1;
the reaction process is as follows:
step S13, mixing phenol, dichloromethane and phosphorus oxychloride, heating to 55 ℃ under the protection of nitrogen, stirring for reaction for 1h, then dropwise adding a dichloromethane solution of triethylamine, continuing stirring for reaction for 4h after dropwise adding, performing vacuum filtration after reaction, performing vacuum concentration on the obtained filtrate, and removing the solvent to obtain an intermediate 3; wherein the dichloromethane solution of triethylamine is triethylamine and dichloromethane are prepared according to the weight ratio of 1g:10mL of the mixture is obtained; the dosage ratio of phenol, dichloromethane, phosphorus oxychloride and triethylamine is 0.02mol:30mL of: 0.01mol:0.02mol;
the reaction process is as follows:
s14, mixing sodium carbonate and deionized water, stirring and dissolving, adding the intermediate 2, stirring for 20min at the temperature of 60 ℃, then adding the intermediate 3, keeping the temperature unchanged after adding, continuing to react for 2h, reducing pressure and filtering after the reaction is finished, washing a filter cake with the deionized water until a washing liquid is neutral, and then recrystallizing with acetone to obtain a flame-retardant component; wherein the dosage ratio of the sodium carbonate, the deionized water, the intermediate 2 and the intermediate 3 is 2.7g:200mL of: 12g:6.7g.
The reaction process is as follows:
further, the average molecular weight of the polyol mixture is 200-600g/mol, the hydroxyl value is 300-800mgKOH/g, and the viscosity at 25 ℃ is 2000-6000mPa & s;
the foaming agent is one of n-pentane, isopentane and cyclopentane;
the catalyst is triethylene diamine;
the cross-linking agent is pentaerythritol and glycerol according to the mass ratio of 1:2-3, mixing;
the polyisocyanate is one of toluene diisocyanate, isophorone diisocyanate and diphenylmethane diisocyanate;
the heat insulation filler is glass wool.
The preparation method of the antistatic heat-insulating plastic pipe comprises the following steps:
firstly, mixing and stirring a polyol mixture, a foaming agent, a catalyst, a cross-linking agent and an additive, and uniformly mixing to obtain a mixture;
secondly, respectively controlling the temperature of the polyisocyanate and the mixture to be 20-35 ℃, adding the polyisocyanate and the heat insulation filler into the mixture at the temperature of 20-35 ℃, then stirring the materials, pouring the materials into a mould for foaming and molding, and then demoulding;
and thirdly, post-curing treatment is carried out after demoulding, wherein the curing temperature of the post-curing treatment is 80-100 ℃, and the curing time is 4-12 hours.
The invention has the beneficial effects that:
the additive is prepared by quaternization reaction of a flame-retardant component and sodium chloroacetate, combines the flame-retardant component with a flame-retardant effect and a quaternary ammonium salt structure to generate synergism, is favorable for improving the atom utilization rate, has good application prospect, plays the flame-retardant and antistatic effects on the premise of not influencing the heat preservation and insulation effects of the antistatic heat-preservation plastic pipe, and has good application prospect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a flame-retardant component:
step S11, adding lauric acid and xylene into a reaction kettle, connecting a water diversion device, adding diethylenetriamine, heating to 140 ℃ until water is separated out, then continuing heating to 240 ℃, reacting until water is not separated out, then cooling to 120 ℃, concentrating under reduced pressure, removing a solvent, then recrystallizing with acetone, and then drying at 40 ℃ to constant weight to obtain an intermediate 1; wherein the dosage ratio of the lauric acid to the diethylenetriamine to the xylene is 0.1mol:0.1mol:30mL;
s12, mixing cyanuric chloride and a solvent, then mixing sodium hydroxide and an aqueous solution of the intermediate 1, adding the mixture, controlling the speed in the adding process, keeping the temperature at 0 ℃ and the pH value at about 6, and reacting for 2 hours to obtain an intermediate 2; wherein the solvent is acetone; aqueous solution of intermediate 1 was intermediate 1 and deionized water according to 13g:20mL of the mixture is mixed; the dosage ratio of cyanuric chloride, solvent and sodium hydroxide is 0.1mol:60mL of: 0.1mmol; the molar ratio of the cyanuric chloride to the intermediate 1 is 1:1;
step S13, mixing phenol, dichloromethane and phosphorus oxychloride, heating to 55 ℃ under the protection of nitrogen, stirring for reaction for 1h, then dropwise adding a dichloromethane solution of triethylamine, continuing stirring for reaction for 4h after dropwise adding, performing vacuum filtration after reaction, performing vacuum concentration on the obtained filtrate, and removing the solvent to obtain an intermediate 3; wherein the dichloromethane solution of triethylamine is triethylamine and dichloromethane, and the weight ratio of triethylamine to dichloromethane is 1g:10mL of the mixture is mixed; the dosage ratio of the phenol, the dichloromethane, the phosphorus oxychloride and the triethylamine is 0.02mol:30mL of: 0.01mol:0.02mol;
s14, mixing sodium carbonate and deionized water, stirring and dissolving, adding the intermediate 2, stirring for 20min at the temperature of 60 ℃, then adding the intermediate 3, keeping the temperature unchanged after adding, continuing to react for 2h, reducing pressure and filtering after the reaction is finished, washing a filter cake with the deionized water until a washing liquid is neutral, and then recrystallizing with acetone to obtain a flame-retardant component; wherein the dosage ratio of the sodium carbonate, the deionized water, the intermediate 2 and the intermediate 3 is 2.7g:200mL of: 12g:6.7g.
Example 2
Preparing an additive:
mixing the flame-retardant component and isopropanol, adding sodium chloroacetate while stirring at the temperature of 80 ℃, adding sodium hydroxide in the reaction process to adjust the pH value to 7, then carrying out heat preservation reaction for 4 hours, and after the reaction is finished, carrying out reduced pressure concentration to remove the solvent to obtain the additive.
Wherein the dosage ratio of the flame-retardant component to the isopropanol is 1g:10mL; the mass ratio of the flame-retardant component to the sodium chloroacetate is 7.5:2.4; the flame retardant component was prepared as in example 1.
Example 3
Mixing the flame-retardant component and isopropanol, adding sodium chloroacetate while stirring at the temperature of 90 ℃, adding sodium hydroxide in the reaction process to adjust the pH value to 9, then carrying out heat preservation reaction for 4 hours, and after the reaction is finished, carrying out reduced pressure concentration to remove the solvent to obtain the additive.
Wherein the dosage ratio of the flame-retardant component to the isopropanol is 1g:10mL; the mass ratio of the flame-retardant component to the sodium chloroacetate is 7.5:2.4; the flame retardant component was prepared as in example 1.
Example 4
Preparing an antistatic heat-insulating plastic pipe:
firstly, mixing and stirring a polyol mixture, a foaming agent, a catalyst, a cross-linking agent and an additive, and uniformly mixing to obtain a mixture;
secondly, respectively controlling the temperature of the polyisocyanate and the mixture to be 20 ℃, adding the polyisocyanate and the heat insulation filler into the mixture at the temperature of 20 ℃, then stirring the materials, pouring the materials into a mould for foaming and molding, and then demoulding;
and step three, performing post-curing treatment after demolding, wherein the curing temperature of the post-curing treatment is 80 ℃, and the curing time is 4 hours.
Wherein the weight parts of each substance are as follows: 80 parts of a polyol mixture, 20 parts of a foaming agent, 1 part of a catalyst, 1 part of a cross-linking agent, 15 parts of an additive, 95 parts of polyisocyanate and 8 parts of a heat-insulating filler;
the foaming agent is n-pentane; the catalyst is triethylene diamine; the cross-linking agent is pentaerythritol and glycerol according to the mass ratio of 1:2, mixing; the polyisocyanate is toluene diisocyanate; the heat insulation filler is glass wool; the additive was prepared as in example 3.
Example 5
Preparing an antistatic heat-insulating plastic pipe:
firstly, mixing and stirring a polyol mixture, a foaming agent, a catalyst, a cross-linking agent and an additive, and uniformly mixing to obtain a mixture;
secondly, respectively controlling the temperature of the polyisocyanate and the mixture to be 25 ℃, adding the polyisocyanate and the heat insulation filler into the mixture at the temperature of 25 ℃, then stirring the materials, pouring the materials into a mould for foaming and molding, and then demoulding;
and thirdly, post-curing treatment is carried out after demoulding, wherein the curing temperature of the post-curing treatment is 90 ℃, and the curing time is 8 hours.
Wherein the weight parts of each substance are as follows: 80 parts of polyol mixture, 25 parts of foaming agent, 2 parts of catalyst, 2 parts of cross-linking agent, 20 parts of additive, 100 parts of polyisocyanate and 10 parts of heat-insulating filler;
the foaming agent is isopentane; the catalyst is triethylene diamine; the cross-linking agent is pentaerythritol and glycerol according to the mass ratio of 1:3, mixing; the polyisocyanate is isophorone diisocyanate; the heat insulation filler is glass wool; the additive was prepared as in example 3.
Example 6
Preparing an antistatic heat-insulating plastic pipe:
firstly, mixing and stirring a polyol mixture, a foaming agent, a catalyst, a cross-linking agent and an additive, and uniformly mixing to obtain a mixture;
secondly, respectively controlling the temperature of the polyisocyanate and the mixture to be 35 ℃, adding the polyisocyanate and the heat insulation filler into the mixture at the temperature of 35 ℃, then stirring the materials, pouring the materials into a mould for foaming and molding, and then demoulding;
and step three, after demolding, performing post-curing treatment, wherein the curing temperature of the post-curing treatment is 100 ℃, and the curing time is 12 hours.
Wherein the weight parts of the substances are as follows: 80 parts of a polyol mixture, 30 parts of a foaming agent, 3 parts of a catalyst, 2 parts of a cross-linking agent, 25 parts of an additive, 100 parts of polyisocyanate and 12 parts of a heat-insulating filler;
the foaming agent is cyclopentane; the catalyst is triethylene diamine; the cross-linking agent is pentaerythritol and glycerol according to the mass ratio of 1:3, mixing; the polyisocyanate is diphenylmethane diisocyanate; the heat insulation filler is glass wool; the additive was prepared as in example 3.
Comparative example 1
The additive of example 5 was replaced by the antistatic agent SH-105, the remaining raw materials and the preparation were kept unchanged.
Comparative example 2
The additives of example 5 were removed and the remaining raw materials and preparation process remained the same.
The samples obtained in examples 4 to 6 and comparative examples 1 to 2 were subjected to the test;
wherein, the heat conductivity coefficient test: the sample size was 200mm X25 mm as determined in accordance with GB/T10294-2008.
And (3) testing an oxygen index: the sample size was 150mm by 10mm, as determined in accordance with GB/T2406.2-2009.
The test results are shown in table 1 below:
TABLE 1
| Example 4 | Example 5 | Example 6 | Comparative example 1 | Comparative example 2 | |
| Surface resistivity/omega | 3.3×10 5 | 3.2×10 5 | 3.2×10 5 | 8.6×10 6 | 3.1×10 8 |
| Coefficient of thermal conductivity W/m | 0.018 | 0.018 | 0.018 | 0.021 | 0.022 |
| Oxygen index/% | 29.4 | 29.8 | 29.7 | 16.5 | 15.4 |
The antistatic heat-insulating plastic pipe prepared by the invention has good antistatic effect and excellent flame retardant property.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The antistatic heat-insulating plastic pipe is characterized by comprising the following raw materials in parts by weight:
80 parts of polyol mixture, 20-30 parts of foaming agent, 1-3 parts of catalyst, 1-2 parts of cross-linking agent, 15-25 parts of additive, 95-100 parts of polyisocyanate and 8-12 parts of heat insulation filler;
the additive is prepared by the following steps:
mixing the flame-retardant component and isopropanol, adding sodium chloroacetate while stirring at the temperature of 80-90 ℃, adding sodium hydroxide in the reaction process to adjust the pH value to 7-9, then carrying out heat preservation reaction for 4 hours, and after the reaction is finished, carrying out reduced pressure concentration to remove the solvent to obtain an additive;
the flame retardant component is prepared by the following steps:
step S11, adding lauric acid and xylene into a reaction kettle, then adding diethylenetriamine, heating to 140 ℃ until water is separated out, then continuing heating to 240 ℃ for reaction until water is not separated out, and obtaining an intermediate 1;
s12, mixing cyanuric chloride and a solvent, then mixing sodium hydroxide and an aqueous solution of the intermediate 1, adding the mixture, controlling the speed in the adding process, keeping the temperature at 0 ℃, and reacting for 2 hours to obtain an intermediate 2;
step S13, mixing phenol, dichloromethane and phosphorus oxychloride, heating to 55 ℃ under the protection of nitrogen, stirring for reacting for 1h, then dropwise adding a dichloromethane solution of triethylamine, and continuing stirring for reacting for 4h after dropwise adding is finished to obtain an intermediate 3;
and S14, mixing sodium carbonate and deionized water, stirring and dissolving, adding the intermediate 2, stirring at 60 ℃ for 20min, adding the intermediate 3, keeping the temperature unchanged after the addition is finished, and continuously reacting for 2h to obtain the flame-retardant component.
2. An antistatic insulation plastic pipe according to claim 1 wherein the ratio of the amount of flame retardant component to the amount of isopropyl alcohol is 1g:10mL; the mass ratio of the flame-retardant component to the sodium chloroacetate is 7.5:2.4.
3. an antistatic insulated plastic pipe according to claim 1 wherein the blowing agent is one of n-pentane, isopentane and cyclopentane.
4. An antistatic insulation plastic pipe according to claim 1 wherein the catalyst is triethylene diamine.
5. An antistatic insulation plastic pipe according to claim 1, characterized in that the cross-linking agent is pentaerythritol and glycerol in a mass ratio of 1:2-3, mixing.
6. An antistatic heat-insulating plastic pipe according to claim 1, characterized in that the polyisocyanate is one of toluene diisocyanate, isophorone diisocyanate and diphenylmethane diisocyanate.
7. An antistatic insulation plastic pipe according to claim 1 wherein the insulating filler is glass wool.
8. The method for preparing an antistatic heat-insulating plastic pipe according to claim 1, comprising the following steps:
firstly, mixing and stirring a polyol mixture, a foaming agent, a catalyst, a cross-linking agent and an additive, and uniformly mixing to obtain a mixture;
secondly, adding the polyisocyanate and the heat insulation filler into the mixture at the temperature of 20-35 ℃, then stirring the materials, pouring the materials into a mould for foaming and forming, and then demoulding;
and thirdly, post-curing treatment is carried out after demoulding, wherein the post-curing temperature is 80-100 ℃, and the curing time is 4-12 hours.
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