CN111662162B - Additive for improving ultraviolet transmittance of coal-made glycol and method for preparing polyester-grade glycol by using additive - Google Patents
Additive for improving ultraviolet transmittance of coal-made glycol and method for preparing polyester-grade glycol by using additive Download PDFInfo
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- CN111662162B CN111662162B CN202010444776.8A CN202010444776A CN111662162B CN 111662162 B CN111662162 B CN 111662162B CN 202010444776 A CN202010444776 A CN 202010444776A CN 111662162 B CN111662162 B CN 111662162B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/94—Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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Abstract
The invention discloses an additive for improving ultraviolet transmittance of coal-made glycol and a method for preparing polyester-grade glycol by using the additive. The additive comprises, by weight, 10-40% of phytic acid and 60-90% of desalted water. Firstly, preparing phytic acid and desalted water according to a proportion; then the mixture is metered into the lower part of a rectifying tower I and reacts with a crude product of the coal-made glycol entering the lower part, and glycol products with the mass more than 99.5 percent are discharged from a tower kettle after the reaction; and (4) treating the discharged product in a rectifying tower II to obtain a mixture of ethylene glycol products meeting the polyester grade index and heavy components and ethylene glycol discharged from the tower bottom. The additive provided by the invention is adopted in the refining process of the coal-to-ethylene glycol, the ultraviolet transmittance of an ethylene glycol product can be greatly increased, the production consumption is reduced, the product yield is remarkably improved, the additive has practical significance and good popularization market prospect, and the overall level of the project reaches the international leading level.
Description
The technical field is as follows:
the invention belongs to the technical field of chemical industry, and particularly relates to an additive for improving ultraviolet transmittance of coal-made glycol and a method for preparing polyester-grade glycol by using the additive.
Secondly, background art:
the ultraviolet light transmittance is an important index for measuring the quality of polyester-grade ethylene glycol products; GB/T4649-2018 "industrial ethylene glycol" stipulates that the ultraviolet light transmittance of ethylene glycol at wavelengths of 220nm, 275nm and 350nm is respectively more than 75%, 92% and 99% when the liquid layer is 10mm thick. The ultraviolet light transmittance can sensitively reflect the quality condition of the glycol, if the quality condition of the glycol does not reach polyester grade, the coloring, strength, color and the like of fiber-grade polyester are influenced, so that the requirement of polyester manufacturers on the ultraviolet light transmittance of the glycol is very strict, part of polyester manufacturers perform enterprise standards on raw material acceptance, and the light transmittance acceptance standards of wavelengths of 220nm, 275nm and 350nm are more than 75%, 95% and 99%.
In order to ensure that the product reaches polyester grade, the process is realized by increasing the amount of the impurity-removing alcohol, the production energy consumption is high, the yield of the glycol is reduced, and the light transmittance of the product is at the edge of the polyester grade index and has a certain difference with the requirement of fiber grade polyester. In order to ensure the grade rate of ethylene glycol polyester, improve the recovery rate of ethylene glycol and improve the competitiveness of coal-made ethylene glycol entering a polyester market, the invention puts the coal-made ethylene glycol ultraviolet transmittance improving additive into a rectification system through the research of self-made ultraviolet transmittance improving additive, improves the ultraviolet transmittance of products, meets the requirements of high-end polyester market, improves the economic benefit of coal-made ethylene glycol and creates a leading position of the same industry technology.
The domestic ethylene glycol refining adopts some special treatment methods to meet the use requirement of polyester-grade ethylene glycol, but the methods are all established on the research of preparing ethylene glycol from petroleum, and the methods are lack of applicability on preparing ethylene glycol from coal.
Thirdly, the invention content:
the technical problem to be solved by the invention is as follows: according to the technical problem of ultraviolet light transmittance of the existing prepared polyester-grade glycol product, the invention provides an additive for improving the ultraviolet light transmittance of coal-made glycol and a method for preparing the polyester-grade glycol by using the additive. The additive adopted by the invention has the advantages of good thermal stability, easy purchase, simple preparation, low cost, environmental protection and the like; the additive provided by the invention is used in the refining process of the coal-to-ethylene glycol, can greatly improve the ultraviolet transmittance of ethylene glycol products, reduce the production consumption, and remarkably improve the product yield, and has practical significance and good popularization market prospect, and the overall level of the project reaches the international leading level.
In order to solve the problems, the invention adopts the technical scheme that:
the invention provides an additive for improving ultraviolet transmittance of coal-made ethylene glycol, which comprises 10-40% of phytic acid and 60-90% of desalted water in percentage by weight.
According to the additive for improving the ultraviolet transmittance of the coal-made glycol, the quality of the phytic acid meets the chemical industry standard HG2683-95 food additive phytic acid (phytic acid), and the mass percentage of the phytic acid is more than or equal to 70%.
According to the additive for improving the ultraviolet transmittance of the coal-made ethylene glycol, the quality of the desalted water meets GB/T6682-2008 'Water specification and test method for analytical laboratories', the conductivity (25 ℃) is less than or equal to 0.50ms/m and more than three levels of water.
In addition, a process for preparing polyester grade ethylene glycol using the above additive is provided, the process comprising the steps of:
a. firstly, weighing phytic acid and desalted water according to the proportion of the additives, and then adding the phytic acid and the desalted water into a storage tank for later use;
b. b, metering the phytic acid and the desalted water prepared in the storage tank in the step a, adding the phytic acid and the desalted water into the lower part of a rectifying tower I, feeding a coal glycol crude product prepared by a conventional method into the rectifying tower I, reacting an additive and the coal glycol crude product in the rectifying tower I, and discharging an ethylene glycol product with the mass of more than 99.5% from a tower kettle after reaction;
(components with boiling points lower than 1, 2-butanediol and 1, 4-butyrolactone are removed from the top of the rectifying tower I, materials with boiling points lower than that of ethylene glycol are further removed and discharged from a tower kettle, and the contents of 1, 2-butanediol and 1, 4-butyrolactone in the tower kettle are less than 0.05%);
c. ethylene glycol products discharged from the tower kettle of the rectifying tower I are pumped into the rectifying tower II from the middle lower part of the rectifying tower II through a pump, part of low-boiling-point components are removed from the tower top of the rectifying tower II, the components are sent into a liquid phase hydrogenation reactor for optimized circulation, ethylene glycol products meeting polyester grade indexes are collected from the side line of the rectifying tower II, and the content of the ethylene glycol is more than 99.9%; the mixture of heavy components and ethylene glycol is discharged from the tower bottom, and the content of the ethylene glycol is more than 90 percent.
According to the method for preparing the polyester-grade ethylene glycol, the crude product of the coal-to-ethylene glycol in the step b contains, by mass, 99.5-99.7% of ethylene glycol, 0.05-0.10% of 1, 2-butanediol, 0.01-0.02% of 1, 4-butyrolactone, 0.01-0.03% of 1, 4-butanediol, 0.01-0.02% of ethylene carbonate, 0.01-0.02% of 1, 2-hexanediol and 0.02-0.03% of water.
According to the method for preparing the polyester-grade ethylene glycol, in the process of adding the phytic acid and the desalted water into the rectifying tower I after metering in the step b, a metering pump with the rated flow of 30L/h is adopted for operation, and the operation flow is 5-30L/h.
According to the method for preparing the polyester-grade ethylene glycol, the metering pump is a diaphragm metering pump (made of stainless steel materials), the flow rate of the diaphragm metering pump is 30L/h, the pressure of the diaphragm metering pump is 0.5MPa, and the operation flow rate of the diaphragm metering pump is 5-30L/h.
According to the method for preparing the polyester-grade ethylene glycol, in the step b, the operating pressure of the rectifying tower I is 20-25 KPa, the temperature of the top of the rectifying tower is 142-150 ℃, the temperature of the bottom of the rectifying tower is 155-165 ℃, and the reflux ratio is 2-3.5.
According to the method for preparing the polyester-grade ethylene glycol, in the step c, the operating pressure of the rectifying tower II is 7-15 KPa, the temperature of the top of the rectifying tower is 135-140 ℃, the temperature of the bottom of the rectifying tower is 144-150 ℃, and the reflux ratio is 1-3.
According to the method for preparing the polyester-grade glycol, the glycol product meeting the polyester-grade index in the step c has the light transmittance of T220nm 85-92%, T275nm 95-98%, T350nm 99.5.5-100.5%, the chromaticity < 5#, the water content less than or equal to 0.05% and the acidity less than or equal to 8 mg/kg.
The invention has the following positive beneficial effects:
1. the additive is added and used in the refining and purifying process of the coal-based glycol, so that the ultraviolet transmittance of the glycol product can be improved, the production consumption is reduced, the product yield is improved from 98% to 99.5%, and the use requirement of a fiber-grade polyester manufacturer is met.
2. The additive adopted by the invention has the advantages of good thermal stability, easy purchase and preparation, low cost, environmental protection and the like, and is suitable for application and popularization in the market.
3. When the additive is applied to the refining process of the coal-to-ethylene glycol, no new impurities are generated in the ethylene glycol product, the purity of the obtained product is more than 99.9 percent, and the requirement of polyester grade is met.
4. According to the technical scheme, the light transmittance and the yield of the product can be improved, and more than 1000 ten thousand yuan of profit can be created for enterprises every year by calculating 20 ten thousand tons per year of the unit ethylene glycol device.
5. The invention can realize safe and environment-friendly operation, improve the recovery rate of glycol products, reduce consumption, improve the competitiveness of coal-to-glycol in polyester markets, has low investment, quick response and convenient operation, and the produced glycol products meet the technical indexes of GB/T4649-2018 and meet the requirements of fiber-grade polyester, and the ultraviolet light transmittance reaches T220nm 85-92%, T275nm 95-98% and T350nm 99.5.5-100.5%.
In conclusion, the invention has obvious economic benefit and social benefit.
The fifth embodiment is as follows:
the invention is further illustrated by the following examples, which do not limit the scope of the invention.
The phytic acid adopted in the following embodiments of the invention meets the chemical industry standard HG 2683-95: "food additive phytic acid (phytic acid)", wherein the mass percentage of the phytic acid is more than or equal to 70%; the quality of the desalted water adopted by the method accords with GB/T6682-2008 'Water specification and test method for analytical laboratories', the conductivity (25 ℃) is less than or equal to 0.50ms/m, and the conductivity is higher than three levels of water.
Example 1:
the additive for improving the ultraviolet transmittance of the coal-made glycol is composed of 12% of phytic acid and 88% of desalted water in percentage by weight.
Example 2:
the additive for improving the ultraviolet transmittance of the coal-made glycol is composed of 25% of phytic acid and 75% of desalted water in percentage by weight.
Example 3:
the additive for improving the ultraviolet transmittance of the coal-made ethylene glycol comprises 36% of phytic acid and 64% of desalted water in percentage by weight.
Example 4:
the additive for improving the ultraviolet transmittance of the coal-made glycol is composed of 40% of phytic acid and 60% of desalted water in percentage by weight.
Example 5:
the additive for improving the ultraviolet transmittance of the coal-made glycol is composed of 10% of phytic acid and 90% of desalted water in percentage by weight.
Example 6:
the invention relates to a method for preparing polyester-grade ethylene glycol by using the additive described in example 1, which comprises the following detailed steps:
a. firstly, weighing 12 percent of phytic acid and 88 percent of desalted water according to the proportion of the additive in the embodiment 1, and then adding the phytic acid and the 88 percent of desalted water into a storage tank for later use;
b. b, metering the phytic acid and the desalted water prepared in the storage tank in the step a, operating by adopting a diaphragm pump metering pump with the rated flow of 25L/h after metering, pumping the additive into the lower part of the rectifying tower I, feeding the coal glycol crude product prepared by the conventional method into the rectifying tower I from the lower part of the rectifying tower I, reacting the additive and the coal glycol crude product in the rectifying tower I, controlling the operating pressure of the rectifying tower I to be 20-25 KPa, the temperature of the top of the rectifying tower to be 142-150 ℃, the temperature of a tower kettle to be 155-165 ℃ and the reflux ratio to be 2-3.5; after the reaction, glycol products with the mass more than 99.5 percent are discharged from the tower kettle;
(components with boiling points lower than 1, 2-butanediol and 1, 4-butyrolactone are removed from the top of the rectifying tower I, materials with boiling points lower than that of ethylene glycol are further removed and discharged from a tower kettle, and the contents of 1, 2-butanediol and 1, 4-butyrolactone in the tower kettle are less than 0.05%);
c. pumping ethylene glycol products discharged from the tower kettle of the rectifying tower I into the rectifying tower II from the middle lower part of the rectifying tower II through a pump, controlling the operating pressure of the rectifying tower II to be 7-15 KPa, controlling the temperature of the tower top to be 135-140 ℃, the temperature of the tower kettle to be 144-150 ℃, the reflux ratio to be 1-3, removing part of low-boiling components from the tower top, feeding the low-boiling components into a liquid phase hydrogenation reactor for optimized circulation, and collecting ethylene glycol products meeting polyester grade indexes from the side line of the rectifying tower II, wherein the content of the ethylene glycol is 99.9%; the mixture of heavy components and ethylene glycol with the ethylene glycol content of 90% is discharged from the bottom of the column.
The light transmittance of the glycol product meeting the polyester grade index obtained in the embodiment is T220nm 85-90%, T275nm 95-97%, T350nm 99.5-100.5%, the chroma is less than # 5, the water content is less than or equal to 0.05%, and the acidity is less than or equal to 5 mg/kg.
Example 7:
the invention relates to a method for preparing polyester-grade ethylene glycol by using the additive described in example 2, which comprises the following detailed steps:
a. firstly, weighing 25 percent of phytic acid and 75 percent of desalted water according to the proportion of the additive in the embodiment 2, and then adding the phytic acid and the desalted water into a storage tank for later use;
b. b, metering the phytic acid and the desalted water prepared in the storage tank in the step a, operating by adopting a diaphragm pump metering pump with the rated flow of 12L/h after metering, pumping the additive into the lower part of the rectifying tower I, feeding the coal glycol crude product prepared by the conventional method into the rectifying tower I from the lower part of the rectifying tower I, reacting the additive and the coal glycol crude product in the rectifying tower I, controlling the operating pressure of the rectifying tower I to be 20-25 KPa, the temperature of the top of the rectifying tower to be 142-150 ℃, the temperature of a tower kettle to be 155-165 ℃ and the reflux ratio to be 2-3.5; after the reaction, glycol products with the mass more than 99.5 percent are discharged from the tower kettle;
(components with boiling points lower than 1, 2-butanediol and 1, 4-butyrolactone are removed from the top of the rectifying tower I, materials with boiling points lower than that of ethylene glycol are further removed and discharged from a tower kettle, and the contents of 1, 2-butanediol and 1, 4-butyrolactone in the tower kettle are less than 0.05%);
c. pumping ethylene glycol products discharged from the tower kettle of the rectifying tower I into the rectifying tower II from the middle lower part of the rectifying tower II through a pump, controlling the operating pressure of the rectifying tower II to be 7-15 KPa, controlling the temperature of the tower top to be 135-140 ℃, the temperature of the tower kettle to be 144-150 ℃, the reflux ratio to be 1-3, removing part of low-boiling components from the tower top, feeding the low-boiling components into a liquid phase hydrogenation reactor for optimized circulation, and collecting ethylene glycol products meeting polyester grade indexes from the side line of the rectifying tower II, wherein the content of the ethylene glycol is 99.9%; the mixture of heavy components and ethylene glycol with the ethylene glycol content of 90% is discharged from the bottom of the column.
The light transmittance of the glycol product meeting the polyester grade index obtained in the embodiment is T220nm 86-91%, T275nm 95-98%, T350nm 99.5-100.5%, the chroma is less than # 5, the water content is less than or equal to 0.04%, and the acidity is less than or equal to 6 mg/kg.
Example 8:
the invention relates to a method for preparing polyester-grade ethylene glycol by using the additive described in example 3, which comprises the following detailed steps:
a. firstly, weighing 36 percent of phytic acid and 64 percent of desalted water according to the proportion of the additive in the embodiment 3, and then adding the phytic acid and the desalted water into a storage tank for later use;
b. b, metering the phytic acid and the desalted water prepared in the storage tank in the step a, operating by adopting a diaphragm pump metering pump with the rated flow of 8L/h after metering, pumping the additive into the lower part of the rectifying tower I, feeding the coal glycol crude product prepared by the conventional method into the rectifying tower I from the lower part of the rectifying tower I, reacting the additive and the coal glycol crude product in the rectifying tower I, controlling the operating pressure of the rectifying tower I to be 20-25 KPa, the temperature of the top of the rectifying tower to be 142-150 ℃, the temperature of a tower kettle to be 155-165 ℃ and the reflux ratio to be 2-3.5; after the reaction, glycol products with the mass more than 99.5 percent are discharged from the tower kettle;
(components with boiling points lower than 1, 2-butanediol and 1, 4-butyrolactone are removed from the top of the rectifying tower I, materials with boiling points lower than that of ethylene glycol are further removed and discharged from a tower kettle, and the contents of 1, 2-butanediol and 1, 4-butyrolactone in the tower kettle are less than 0.05%);
c. pumping ethylene glycol products discharged from the tower kettle of the rectifying tower I into the rectifying tower II from the middle lower part of the rectifying tower II through a pump, controlling the operating pressure of the rectifying tower II to be 7-15 KPa, controlling the temperature of the tower top to be 135-140 ℃, the temperature of the tower kettle to be 144-150 ℃, the reflux ratio to be 1-3, removing part of low-boiling components from the tower top, feeding the low-boiling components into a liquid phase hydrogenation reactor for optimized circulation, and collecting ethylene glycol products meeting polyester grade indexes from the side line of the rectifying tower II, wherein the content of the ethylene glycol is 99.9%; the mixture of heavy components and ethylene glycol with the ethylene glycol content of 90% is discharged from the bottom of the column.
The light transmittance of the glycol product meeting the polyester grade index obtained in the embodiment is T220nm 87-92%, T275nm 96-98%, T350nm 99.5-100.5%, the chroma is less than # 5, the water content is less than or equal to 0.03%, and the acidity is less than or equal to 7 mg/kg.
Example 9:
the invention relates to a method for preparing polyester-grade ethylene glycol by using the additive described in example 4, which comprises the following detailed steps:
a. firstly, weighing 40 percent of phytic acid and 60 percent of desalted water according to the proportion of the additive in the embodiment 4, and then adding the phytic acid and the desalted water into a storage tank for later use;
b. b, metering the phytic acid and the desalted water prepared in the storage tank in the step a, operating by adopting a diaphragm pump metering pump with the rated flow of 20L/h after metering, pumping the additive into the lower part of the rectifying tower I, feeding the coal glycol crude product prepared by the conventional method into the rectifying tower I from the lower part of the rectifying tower I, reacting the additive and the coal glycol crude product in the rectifying tower I, controlling the operating pressure of the rectifying tower I to be 20-25 KPa, the temperature of the top of the rectifying tower to be 142-150 ℃, the temperature of a tower kettle to be 155-165 ℃ and the reflux ratio to be 2-3.5; after the reaction, glycol products with the mass more than 99.5 percent are discharged from the tower kettle;
(components with boiling points lower than 1, 2-butanediol and 1, 4-butyrolactone are removed from the top of the rectifying tower I, materials with boiling points lower than that of ethylene glycol are further removed and discharged from a tower kettle, and the contents of 1, 2-butanediol and 1, 4-butyrolactone in the tower kettle are less than 0.05%);
c. pumping ethylene glycol products discharged from the tower kettle of the rectifying tower I into the rectifying tower II from the middle lower part of the rectifying tower II through a pump, controlling the operating pressure of the rectifying tower II to be 7-15 KPa, controlling the temperature of the tower top to be 135-140 ℃, the temperature of the tower kettle to be 144-150 ℃, the reflux ratio to be 1-3, removing part of low-boiling components from the tower top, feeding the low-boiling components into a liquid phase hydrogenation reactor for optimized circulation, and collecting ethylene glycol products meeting polyester grade indexes from the side line of the rectifying tower II, wherein the content of the ethylene glycol is 99.9%; the mixture of heavy components and ethylene glycol with the ethylene glycol content of 90% is discharged from the bottom of the column.
The glycol product meeting the polyester grade index obtained in the embodiment has the light transmittance of T220nm 87-92%, T275nm 96-98%, T350nm 99.5.5-100.5%, the chromaticity less than 5#, the water content less than or equal to 0.03% and the acidity less than or equal to 7 mg/kg.
Example 10:
the invention relates to a method for preparing polyester-grade ethylene glycol by using the additive described in example 5, which comprises the following detailed steps:
a. firstly, weighing 10 percent of phytic acid and 90 percent of desalted water according to the proportion of the additive in the embodiment 5, and then adding the phytic acid and the desalted water into a storage tank for later use;
b. b, metering the phytic acid and the desalted water prepared in the storage tank in the step a, operating by adopting a diaphragm pump metering pump with rated flow of 30L/h after metering, pumping the additive into the lower part of the rectifying tower I, feeding the coal glycol crude product prepared by the conventional method into the rectifying tower I from the lower part of the rectifying tower I, reacting the additive and the coal glycol crude product in the rectifying tower I, controlling the operating pressure of the rectifying tower I to be 20-25 KPa, the temperature of the top of the rectifying tower to be 142-150 ℃, the temperature of a tower kettle to be 155-165 ℃ and the reflux ratio to be 2-3.5; after the reaction, glycol products with the mass more than 99.5 percent are discharged from the tower kettle;
(components with boiling points lower than 1, 2-butanediol and 1, 4-butyrolactone are removed from the top of the rectifying tower I, materials with boiling points lower than that of ethylene glycol are further removed and discharged from a tower kettle, and the contents of 1, 2-butanediol and 1, 4-butyrolactone in the tower kettle are less than 0.05%);
c. pumping ethylene glycol products discharged from the tower kettle of the rectifying tower I into the rectifying tower II from the middle lower part of the rectifying tower II through a pump, controlling the operating pressure of the rectifying tower II to be 7-15 KPa, controlling the temperature of the tower top to be 135-140 ℃, the temperature of the tower kettle to be 144-150 ℃, the reflux ratio to be 1-3, removing part of low-boiling components from the tower top, feeding the low-boiling components into a liquid phase hydrogenation reactor for optimized circulation, and collecting ethylene glycol products meeting polyester grade indexes from the side line of the rectifying tower II, wherein the content of the ethylene glycol is 99.9%; the mixture of heavy components and ethylene glycol with the ethylene glycol content of 90% is discharged from the bottom of the column.
The light transmittance of the glycol product meeting the polyester grade index obtained in the embodiment is T220nm 85-90%, T275nm 95-97%, T350nm 99.5-100.5%, the chroma is less than # 5, the water content is less than or equal to 0.05%, and the acidity is less than or equal to 5 mg/kg.
Claims (10)
1. An additive for improving the ultraviolet transmittance of coal-made ethylene glycol is characterized in that: the additive comprises, by weight, 10-40% of phytic acid and 60-90% of desalted water.
2. The additive for improving the ultraviolet transmittance of coal-made glycol according to claim 1, wherein: the quality of the phytic acid meets chemical industry standard HG2683-95 food additive phytic acid (phytic acid), and the mass percentage of the phytic acid is more than or equal to 70%.
3. The additive for improving the ultraviolet transmittance of coal-made glycol according to claim 1, wherein: the quality of the desalted water accords with GB/T6682-2008 'specification and test method for water for analytical laboratories', the conductivity (25 ℃) is less than or equal to 0.50ms/m above three-level water.
4. A process for preparing polyester grade ethylene glycol using the additive of claim 1, comprising the steps of:
a. firstly, weighing phytic acid and desalted water according to the proportion of the additive in the claim 1, and then adding the phytic acid and the desalted water into a storage tank for later use;
b. b, metering the phytic acid and the desalted water prepared in the storage tank in the step a, adding the phytic acid and the desalted water into the lower part of a rectifying tower I, feeding a coal glycol crude product prepared by a conventional method into the rectifying tower I, reacting an additive and the coal glycol crude product in the rectifying tower I, and discharging an ethylene glycol product with the mass of more than 99.5% from a tower kettle after reaction;
c. ethylene glycol products discharged from the tower kettle of the rectifying tower I are pumped into the rectifying tower II from the middle lower part of the rectifying tower II through a pump, part of low-boiling-point components are removed from the tower top of the rectifying tower II, the components are sent into a liquid phase hydrogenation reactor for optimized circulation, ethylene glycol products meeting polyester grade indexes are collected from the side line of the rectifying tower II, and the content of the ethylene glycol is more than 99.9%; the mixture of heavy components and ethylene glycol is discharged from the tower bottom, and the content of the ethylene glycol is more than 90 percent.
5. The process of claim 4 for the preparation of polyester grade ethylene glycol, characterized in that: the crude product of the coal-derived ethylene glycol in the step b comprises 99.5-99.7% of ethylene glycol, 0.05-0.10% of 1, 2-butanediol, 0.01-0.02% of 1, 4-butyrolactone, 0.01-0.03% of 1, 4-butanediol, 0.01-0.02% of ethylene carbonate, 0.01-0.02% of 1, 2-hexanediol and 0.02-0.03% of water by mass percentage.
6. The process of claim 4 for the preparation of polyester grade ethylene glycol, characterized in that: and b, metering the phytic acid and the desalted water in the step b, and then adding the phytic acid and the desalted water into the rectifying tower I, wherein a metering pump with rated flow of 30L/h is adopted for operation, and the operation flow is 5-30L/h.
7. The process of claim 6, wherein the polyester grade ethylene glycol comprises: the metering pump is a diaphragm metering pump, the flow rate of the diaphragm metering pump is 30L/h, the pressure is 0.5MPa, and the operation flow rate is 5-30L/h.
8. The process of claim 4 for the preparation of polyester grade ethylene glycol, characterized in that: in the step b, the operating pressure of the rectifying tower I is 20-25 KPa, the temperature of the top of the rectifying tower is 142-150 ℃, the temperature of the bottom of the rectifying tower is 155-165 ℃, and the reflux ratio is 2-3.5.
9. The process of claim 4 for the preparation of polyester grade ethylene glycol, characterized in that: in the step c, the operating pressure of the rectifying tower II is 7-15 KPa, the temperature of the top of the tower is 135-140 ℃, the temperature of the bottom of the tower is 144-150 ℃, and the reflux ratio is 1-3.
10. The process of claim 4 for preparing polyester grade ethylene glycol, wherein: the light transmittance of the glycol product meeting the polyester grade index in the step c is T220nm 85-92%, T275nm 95-98%, T350nm 99.5.5-100.5%, the chroma is less than # 5, the water content is less than or equal to 0.05%, and the acidity is less than or equal to 8 mg/kg.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010444776.8A CN111662162B (en) | 2020-05-23 | 2020-05-23 | Additive for improving ultraviolet transmittance of coal-made glycol and method for preparing polyester-grade glycol by using additive |
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| CN202010444776.8A CN111662162B (en) | 2020-05-23 | 2020-05-23 | Additive for improving ultraviolet transmittance of coal-made glycol and method for preparing polyester-grade glycol by using additive |
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| CN111662162A CN111662162A (en) | 2020-09-15 |
| CN111662162B true CN111662162B (en) | 2022-08-12 |
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