CN110590553A - Method for synthesizing dipolyester by using fatty acid methyl ester - Google Patents
Method for synthesizing dipolyester by using fatty acid methyl ester Download PDFInfo
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- CN110590553A CN110590553A CN201910868150.7A CN201910868150A CN110590553A CN 110590553 A CN110590553 A CN 110590553A CN 201910868150 A CN201910868150 A CN 201910868150A CN 110590553 A CN110590553 A CN 110590553A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/333—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton
- C07C67/343—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
- C07C67/347—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by addition to unsaturated carbon-to-carbon bonds
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Abstract
The invention discloses a method for synthesizing a copolyester by using fatty acid methyl ester, which comprises the steps of carrying out operation of high iodine value fatty acid methyl ester in a reaction kettle, then carrying out molecular distillation, then the waste argil is used for extracting the secondary polyester, and finally the materials are fully reacted in a distillation tower, in the invention, two sets of separation and distillation equipment are added in the processing process, so that the primary fractional distillation can be carried out in the first set of separation and distillation equipment, then the light molecules are separated by a second set of separation and distillation equipment, the light molecules reach a condensing plate and are condensed and discharged, the heavy molecules can not reach the condensing plate and are discharged along the mixed liquid, thus achieving the purpose of separating the substances, thereby achieving better separation phenomenon, avoiding waste phenomenon and being capable of being well utilized, thereby solving the problem that the prior dimeric ester may be incompletely separated to cause waste during the molecular distillation of synthesis.
Description
Technical Field
The invention belongs to the technical field related to the synthesis of high molecular polymers, and particularly relates to a method for synthesizing a copolyester by using fatty acid methyl ester.
Background
The fatty acid methyl ester is formed by methylation of fatty acid. Biodiesel is mainly composed of fatty acid methyl esters. In biochemistry, in order to analyze the content of various fatty acids in a sample, lipids in the sample are extracted, the sample is modified into FAMEs by a methylating agent such as BSTFA, the FAMEs can be separated, the content is measured, the isotopic abundance is judged and the like by a gas chromatography, and fatty acid methyl esters can be divided into unsaturated fatty acid methyl esters containing double bonds and saturated fatty acid methyl esters containing no double bonds or triple bonds according to the saturation degree of a carbon chain. The main use of saturated fatty acid methyl esters is the production of the aforementioned surfactants. The unsaturated fatty acid methyl ester can be used for producing the epoxy fatty acid methyl ester besides the surfactant. The latter is an important plasticizer, is widely used for plasticizing resins such as polyvinyl chloride and the like, and can partially replace phthalate plasticizers.
The prior art method for synthesizing the dipolyester has the following problems: the existing dipolyester needs to be distilled by molecular distillation equipment in the synthesis process, so that better extraction can be carried out, but when the distillation equipment is used, a good phase separation effect cannot be achieved, so that the problem of incomplete separation can be caused.
Disclosure of Invention
The invention aims to provide a method for synthesizing a diester by using fatty acid methyl ester, which solves the problem that the prior diester proposed in the background art can cause the phenomenon of incomplete separation and waste during the molecular distillation of synthesis.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for synthesizing a diester by using fatty acid methyl ester, wherein the operation steps of the diester in a synthesis reaction kettle are as follows:
the method comprises the following steps: preparing raw materials, namely high-iodine-value fatty acid methyl ester, wherein the iodine value is more than 130mgI/100g, and anhydrous and impurity-free raw materials are used as main raw materials, and preparing catalyst activated clay;
step two: pumping fatty acid methyl ester with high iodine value into a reaction kettle, and adding activated clay which is 10-15% of the weight of oil;
step three: starting stirring at the stirring speed of 60-80 rpm, introducing nitrogen for protection, slowly heating to 200 ℃ and 250 ℃, and reacting for 8-12 hours;
step four: after the reaction is finished, cooling to 80-120 ℃, centrifuging by a horizontal screw centrifuge to obtain argil, and feeding the dimeric ester crude product into a crude product storage tank. The separated oil-containing white clay residue enters a waste white clay bin;
preferably, the molecular distillation refining of the copolyester comprises the following steps:
the method comprises the following steps: preparing raw materials, and taking a dimer ester crude product as a main raw material;
step two: starting the molecular distillation equipment, and starting a vacuum system and a pipeline until the vacuum degree in the molecular distillation equipment reaches 3-10 Pa;
step three: the pretreated crude oil is heated and then sent into a primary distillation tower of an atmospheric distillation device, and most of light gasoline is distilled. Heating crude oil at the bottom of the primary distillation tower to 360-370 ℃, feeding the crude oil into an atmospheric distillation tower (the number of tower plates is 36-48), wherein the product at the top of the tower is gasoline fraction (also called naphtha), and the gasoline fraction and light gasoline at the top of the primary distillation tower can be used as catalytic reforming raw materials, or petrochemical raw materials, or gasoline blending components. And (3) discharging a side line of the normal pressure tower, feeding the discharged material into a stripping tower, heating by using steam or a reboiler, and evaporating light components to control the content of the light components. Generally, the first lateral line is jet fuel or kerosene fraction, the second lateral line is light diesel oil fraction, the third lateral line is heavy diesel oil or transformer oil fraction (belonging to lubricating oil fraction), and the bottom product is atmospheric residue;
step four: the crude dimer ester product is subjected to heat exchange and heating by a heater, the temperature is controlled at 180 ℃, and the crude dimer ester product enters an air separation tank to separate out trace gas impurities;
step five: the heated crude dimeric ester enters a molecular distillation system, the temperature is controlled at 200 ℃ and 250 ℃, and the vacuum is controlled at 3-10 Pa;
step six: when the liquid mixture flows along the heating plate and is heated, light and heavy molecules can escape from the liquid surface and enter the gas phase, because of different free paths of the light and heavy molecules, the molecules of different substances move for different distances after escaping from the liquid surface, if a condensing plate can be properly arranged, the light molecules reach the condensing plate and are condensed and discharged, and the heavy molecules cannot reach the condensing plate and are discharged along the mixed liquid. Thus, the purpose of material separation is achieved;
step seven: passing through a molecular distillation system, and obtaining a dimer ester product in a heavy phase. And the light-phase unreacted fatty acid methyl ester can be sold as biodiesel.
Preferably, the operation steps of extracting the copolyester from the spent bleaching clay are as follows:
the method comprises the following steps: taking waste argil generated in production as a main raw material, and taking n-hexane as an auxiliary material;
step two: leaching for the first time, wherein the normal hexane accounts for 300 percent of the weight of the waste argil, stirring is started, the stirring speed is 60-80 r/min, and the waste argil is slowly added at normal temperature and normal pressure;
step three: stirring for a while, filtering the waste argil by a vertical filter, and waiting for the removal of the solvent from the liquid phase;
step four: secondary leaching, filtering the waste argil by using a filter, wherein the normal hexane accounts for 300 percent of the weight of the waste argil, starting stirring at the stirring speed of 60-80 rpm, and slowly adding the waste argil at normal temperature and normal pressure;
step five: stirring for a short time, filtering out the waste argil by a vertical filter, and waiting for the removal of the solvent from the liquid phase. The waste argil enters a leaching waste argil bin to be steamed and removed;
step six: adding the liquid phase generated in the fifth step, the second step and the fourth step at 60-80 ℃, removing the solvent through normal-pressure flash evaporation, and recycling the solvent through chilled water;
step seven: and (3) carrying out normal-pressure flash evaporation on the liquid phase after the solvent is removed, carrying out secondary normal-pressure flash evaporation, controlling the temperature to be 80-150 ℃, and completely steaming the n-hexane in the oil phase to obtain a crude dimeric ester product. The crude product is mixed with the crude product after the reaction is finished, and a dimeric ester product can be obtained through molecular distillation. The solvent is used by multi-stage refrigeration water cooling circulation.
Preferably, the operation steps of the materials in the distillation tower are as follows:
the method comprises the following steps: raw materials: the leached waste argil and auxiliary materials are as follows: steam;
step two: continuously adding the waste clay into a distillation tower, and adding a small amount of steam, wherein the steam amount is 0.5-2% of the clay amount;
step three: controlling the temperature of the waste clay at 160 ℃ of 100-;
step four: the evaporated solvent is cooled by chilled water and enters a precipitation tank to separate water, and the obtained solvent n-hexane is recycled;
step five: and (4) performing solid waste treatment on the argil discharged from the inside of the steam stripping tower.
Compared with the prior art, the invention provides a method for synthesizing a copolyester by using fatty acid methyl ester, which has the following beneficial effects:
according to the invention, two sets of separation and distillation equipment are added in the processing process, so that the primary separation and distillation can be carried out in the first set of separation and distillation equipment, then the separation is carried out through the second set of separation and distillation equipment, the light molecules reach the condensing plate and are condensed and discharged, and the heavy molecules cannot reach the condensing plate and are discharged along the mixed liquid, so that the purpose of substance separation is achieved, a better separation phenomenon can be achieved, a waste phenomenon is avoided, the good utilization can be realized, and the problem that the waste phenomenon is caused by incomplete separation in the molecular distillation of the synthesis of the existing polyester is solved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a technical scheme that:
a method for synthesizing a diester by using fatty acid methyl ester, wherein the operation steps of the diester in a synthesis reaction kettle are as follows:
the method comprises the following steps: preparing raw materials, namely high-iodine-value fatty acid methyl ester, wherein the iodine value is more than 130mgI/100g, and anhydrous and impurity-free raw materials are used as main raw materials, and preparing catalyst activated clay;
step two: pumping fatty acid methyl ester with high iodine value into a reaction kettle, and adding activated clay which is 10-15% of the weight of oil;
step three: starting stirring at the stirring speed of 60-80 rpm, introducing nitrogen for protection, slowly heating to 200 ℃ and 250 ℃, and reacting for 8-12 hours;
step four: after the reaction is finished, cooling to 80-120 ℃, centrifuging by a horizontal screw centrifuge to obtain argil, and feeding the dimeric ester crude product into a crude product storage tank. The separated oil-containing white clay residue enters a waste white clay bin;
the operation steps of refining the copolyester by molecular distillation are as follows:
the method comprises the following steps: preparing raw materials, and taking a dimer ester crude product as a main raw material;
step two: starting the molecular distillation equipment, and starting a vacuum system and a pipeline until the vacuum degree in the molecular distillation equipment reaches 3-10 Pa;
step three: the pretreated crude oil is heated and then sent into a primary distillation tower of an atmospheric distillation device, and most of light gasoline is distilled. Heating crude oil at the bottom of the primary distillation tower to 360-370 ℃, feeding the crude oil into an atmospheric distillation tower (the number of tower plates is 36-48), wherein the product at the top of the tower is gasoline fraction (also called naphtha), and the gasoline fraction and light gasoline at the top of the primary distillation tower can be used as catalytic reforming raw materials, or petrochemical raw materials, or gasoline blending components. And (3) discharging a side line of the normal pressure tower, feeding the discharged material into a stripping tower, heating by using steam or a reboiler, and evaporating light components to control the content of the light components. Generally, the first lateral line is jet fuel or kerosene fraction, the second lateral line is light diesel oil fraction, the third lateral line is heavy diesel oil or transformer oil fraction (belonging to lubricating oil fraction), and the bottom product is atmospheric residue;
step four: the crude dimer ester product is subjected to heat exchange and heating by a heater, the temperature is controlled at 180 ℃, and the crude dimer ester product enters an air separation tank to separate out trace gas impurities;
step five: the heated crude dimeric ester enters a molecular distillation system, the temperature is controlled at 200 ℃ and 250 ℃, and the vacuum is controlled at 3-10 Pa;
step six: when the liquid mixture flows along the heating plate and is heated, light and heavy molecules can escape from the liquid surface and enter the gas phase, because of different free paths of the light and heavy molecules, the molecules of different substances move for different distances after escaping from the liquid surface, if a condensing plate can be properly arranged, the light molecules reach the condensing plate and are condensed and discharged, and the heavy molecules cannot reach the condensing plate and are discharged along the mixed liquid. Thus, the purpose of material separation is achieved;
step seven: passing through a molecular distillation system, and obtaining a dimer ester product in a heavy phase. And the light-phase unreacted fatty acid methyl ester can be sold as biodiesel.
The operation steps for extracting the dipolyester from the waste argil are as follows:
the method comprises the following steps: taking waste argil generated in production as a main raw material, and taking n-hexane as an auxiliary material;
step two: leaching for the first time, wherein the normal hexane accounts for 300 percent of the weight of the waste argil, stirring is started, the stirring speed is 60-80 r/min, and the waste argil is slowly added at normal temperature and normal pressure;
step three: stirring for a while, filtering the waste argil by a vertical filter, and waiting for the removal of the solvent from the liquid phase;
step four: secondary leaching, filtering the waste argil by using a filter, wherein the normal hexane accounts for 300 percent of the weight of the waste argil, starting stirring at the stirring speed of 60-80 rpm, and slowly adding the waste argil at normal temperature and normal pressure;
step five: stirring for a short time, filtering out the waste argil by a vertical filter, and waiting for the removal of the solvent from the liquid phase. The waste argil enters a leaching waste argil bin to be steamed and removed;
step six: adding the liquid phase generated in the fifth step, the second step and the fourth step at 60-80 ℃, removing the solvent through normal-pressure flash evaporation, and recycling the solvent through chilled water;
step seven: and (3) carrying out normal-pressure flash evaporation on the liquid phase after the solvent is removed, carrying out secondary normal-pressure flash evaporation, controlling the temperature to be 80-150 ℃, and completely steaming the n-hexane in the oil phase to obtain a crude dimeric ester product. The crude product is mixed with the crude product after the reaction is finished, and a dimeric ester product can be obtained through molecular distillation. The solvent is used by multi-stage refrigeration water cooling circulation.
The operation steps of the materials in the distillation tower are as follows:
the method comprises the following steps: raw materials: the leached waste argil and auxiliary materials are as follows: steam;
step two: continuously adding the waste clay into a distillation tower, and adding a small amount of steam, wherein the steam amount is 0.5-2% of the clay amount;
step three: controlling the temperature of the waste clay at 160 ℃ of 100-;
step four: the evaporated solvent is cooled by chilled water and enters a precipitation tank to separate water, and the obtained solvent n-hexane is recycled;
step five: and (4) performing solid waste treatment on the argil discharged from the inside of the steam stripping tower.
The working principle and the using process of the invention are as follows:
the method comprises the following steps: preparing raw materials, namely high-iodine-value fatty acid methyl ester, wherein the iodine value is more than 130mgI/100g, and anhydrous and impurity-free raw materials are used as main raw materials, and preparing catalyst activated clay;
step two: pumping fatty acid methyl ester with high iodine value into a reaction kettle, and adding activated clay which is 10-15% of the weight of oil;
step three: starting stirring at the stirring speed of 60-80 rpm, introducing nitrogen for protection, slowly heating to 200 ℃ and 250 ℃, and reacting for 8-12 hours;
step four: after the reaction is finished, cooling to 80-120 ℃, centrifuging by a horizontal screw centrifuge to obtain argil, and feeding the dimeric ester crude product into a crude product storage tank. The separated oil-containing white clay residue enters a waste white clay bin;
step five: starting the molecular distillation equipment, and starting a vacuum system and a pipeline until the vacuum degree in the molecular distillation equipment reaches 3-10 Pa;
step six: the crude dimer ester product is subjected to heat exchange and heating by a heater, the temperature is controlled at 180 ℃, and the crude dimer ester product enters an air separation tank to separate out trace gas impurities;
step seven: the heated crude dimeric ester enters a molecular distillation system, the temperature is controlled at 200 ℃ and 250 ℃, and the vacuum is controlled at 3-10 Pa;
step eight: when the liquid mixture flows along the heating plate and is heated, light and heavy molecules can escape from the liquid surface and enter the gas phase, because of different free paths of the light and heavy molecules, the molecules of different substances move for different distances after escaping from the liquid surface, if a condensing plate can be properly arranged, the light molecules reach the condensing plate and are condensed and discharged, and the heavy molecules cannot reach the condensing plate and are discharged along the mixed liquid. Thus, the purpose of material separation is achieved;
step nine: passing through a molecular distillation system, and obtaining a dimer ester product in a heavy phase. And the light-phase unreacted fatty acid methyl ester can be sold as biodiesel.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A method for synthesizing a copolyester by using fatty acid methyl ester is characterized by comprising the following steps: the operation steps of the copolyester in the synthesis reaction kettle are as follows:
the method comprises the following steps: preparing raw materials, namely high-iodine-value fatty acid methyl ester, wherein the iodine value is more than 130mgI/100g, and anhydrous and impurity-free raw materials are used as main raw materials, and preparing catalyst activated clay;
step two: pumping fatty acid methyl ester with high iodine value into a reaction kettle, and adding activated clay which is 10-15% of the weight of oil;
step three: starting stirring at the stirring speed of 60-80 rpm, introducing nitrogen for protection, slowly heating to 200 ℃ and 250 ℃, and reacting for 8-12 hours;
step four: after the reaction is finished, cooling to 80-120 ℃, centrifuging by a horizontal screw centrifuge to obtain argil, and feeding the dimeric ester crude product into a crude product storage tank. The separated oil-containing white clay residue enters a waste white clay bin.
2. The method for synthesizing the di-polyester by using the fatty acid methyl ester as claimed in claim 1, wherein: the operation steps of the molecular distillation refining of the copolyester are as follows:
the method comprises the following steps: preparing raw materials, and taking a dimer ester crude product as a main raw material;
step two: starting the molecular distillation equipment, and starting a vacuum system and a pipeline until the vacuum degree in the molecular distillation equipment reaches 3-10 Pa;
step three: the pretreated crude oil is heated and then sent into a primary distillation tower of an atmospheric distillation device, and most of light gasoline is distilled. Heating crude oil at the bottom of the primary distillation tower to 360-370 ℃, feeding the crude oil into an atmospheric distillation tower (the number of tower plates is 36-48), wherein the product at the top of the tower is gasoline fraction (also called naphtha), and the gasoline fraction and light gasoline at the top of the primary distillation tower can be used as catalytic reforming raw materials, or as petrochemical raw materials, or as gasoline blending components. And (3) discharging a side line of the normal pressure tower, feeding the discharged material into a stripping tower, heating by using steam or a reboiler, and evaporating light components to control the content of the light components. Generally, the first lateral line is jet fuel or kerosene fraction, the second lateral line is light diesel oil fraction, the third lateral line is heavy diesel oil or transformer oil fraction (belonging to lubricating oil fraction), and the bottom product is atmospheric residue;
step four: the crude dimer ester product is subjected to heat exchange and heating by a heater, the temperature is controlled at 180 ℃, and the crude dimer ester product enters an air separation tank to separate out trace gas impurities;
step five: the heated crude dimeric ester enters a molecular distillation system, the temperature is controlled at 200 ℃ and 250 ℃, and the vacuum is controlled at 3-10 Pa;
step six: when the liquid mixture flows along the heating plate and is heated, light and heavy molecules can escape from the liquid surface and enter the gas phase, because of different free paths of the light and heavy molecules, the molecules of different substances move for different distances after escaping from the liquid surface, if a condensing plate can be properly arranged, the light molecules reach the condensing plate and are condensed and discharged, and the heavy molecules cannot reach the condensing plate and are discharged along the mixed liquid. Thus, the purpose of separating substances is achieved;
step seven: passing through a molecular distillation system, and obtaining a dimer ester product in a heavy phase. And the light-phase unreacted fatty acid methyl ester can be sold as biodiesel.
3. The method for synthesizing the di-polyester by using the fatty acid methyl ester as claimed in claim 1, wherein: the operation steps of extracting the dipolyester from the waste argil are as follows:
the method comprises the following steps: taking waste argil generated in production as a main raw material, and taking n-hexane as an auxiliary material;
step two: leaching for the first time, wherein the normal hexane accounts for 300 percent of the weight of the waste argil, stirring is started, the stirring speed is 60-80 r/min, and the waste argil is slowly added at normal temperature and normal pressure;
step three: stirring for a while, filtering the waste argil by a vertical filter, and waiting for the removal of the solvent from the liquid phase;
step four: secondary leaching, filtering the waste argil by using a filter, wherein the normal hexane accounts for 300 percent of the weight of the waste argil, starting stirring at the stirring speed of 60-80 rpm, and slowly adding the waste argil at normal temperature and normal pressure;
step five: stirring for a short time, filtering out the waste argil by a vertical filter, and waiting for the removal of the solvent from the liquid phase. The waste argil enters a leaching waste argil bin to be steamed and removed;
step six: adding the liquid phase generated in the fifth step, the second step and the fourth step at 60-80 ℃, removing the solvent through normal-pressure flash evaporation, and recycling the solvent through chilled water;
step seven: and (3) carrying out normal-pressure flash evaporation on the liquid phase after the solvent is removed, carrying out secondary normal-pressure flash evaporation, controlling the temperature to be 80-150 ℃, and completely steaming the n-hexane in the oil phase to obtain a crude dimeric ester product. The crude product is mixed with the crude product after the reaction, and a dimeric ester product can be obtained through molecular distillation. The solvent is cooled and recycled by multi-stage freezing water.
4. The method for synthesizing the di-polyester by using the fatty acid methyl ester as claimed in claim 1, wherein: the operation steps of the materials in the distillation tower are as follows:
the method comprises the following steps: raw materials: the leached waste argil and auxiliary materials are as follows: steam;
step two: continuously adding the waste clay into a distillation tower, and adding a small amount of steam, wherein the steam amount is 0.5-2% of the clay amount;
step three: controlling the temperature of the waste clay at 160 ℃ of 100-;
step four: the evaporated solvent is cooled by chilled water and enters a precipitation tank to separate water, and the obtained solvent n-hexane is recycled;
step five: and (4) performing solid waste treatment on the argil discharged from the inside of the steam stripping tower.
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