CN218871293U - Benzene diphenol separation and purification system that phenol, hydrogen peroxide solution reaction were prepared - Google Patents
Benzene diphenol separation and purification system that phenol, hydrogen peroxide solution reaction were prepared Download PDFInfo
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Abstract
The utility model provides a system for separating and purifying benzenediol prepared by reacting phenol and hydrogen peroxide, which comprises a phenol dehydrating tower, a phenol dehydrating tower and a phenol mixing tower which are connected in series; the bottom of the dephenolizing tower is sequentially connected with a scraper evaporator and a spiral tar carbonizing machine; the top parts of the scraper evaporator and the spiral tar carbonizing machine are connected with a phenol mixing tower; the top of the phenol mixing tower is connected with a catechol refining tower, and the bottom of the phenol mixing tower is connected with a hydroquinone refining tower; the top of the hydroquinone refining tower is connected with the resorcinol refining tower, and the bottom of the hydroquinone refining tower is connected with the scraper evaporator; the top of the resorcinol refining tower and the bottom of the catechol refining tower are respectively connected with the phenol mixing tower. When separation and purification are carried out, the reaction liquid is subjected to dehydration and dephenolization, evaporation, decoking, catechol refining, hydroquinone refining and resorcinol refining in sequence, the product energy consumption is reduced through the working procedures, the product requirements of high-end customers in the market are met, and the simple operation and stable production are ensured.
Description
Technical Field
The utility model belongs to the technical field of chemical separation, concretely relates to benzenediol separation and purification system and method that phenol, hydrogen peroxide solution reacted and prepared.
Background
Benzenediol of the formula C 6 H 6 O 2 The compound has three isomers of ortho, meta and para, the three isomers are all used as important chemical raw materials and intermediates, and the application field is wide:
catechol is also known as catechol, is a compound formed by substituting two ortho-hydrogens of benzene by hydroxyl, is an important basic organic chemical raw material and an important intermediate in the pharmaceutical industry, is widely used for producing dyes, light stabilizers, photosensitive materials, perfumes, preservatives, accelerators, special inks, electroplating materials and raw lacquer flame retardants, and is also an astringent and an antioxidant which are widely used; can be used for preparing berberine and isopropylene in medicine.
Hydroquinone is also called hydroquinone, is a compound formed by replacing two ortho-hydrogens of benzene with hydroxyl, is used in the fields of manufacturing dyes, medical intermediates, photographic developers, antioxidants, plastic resin polymerization inhibitors and the like, can also interfere with the formation of melanin, and has fading and fading effects on freckles, age spots and liver spots induced by oral contraceptives clinically.
Resorcinol, also known as resorcinol and resorcinol, is a compound formed by substituting two hydrogens at the benzene meta position with a hydroxyl group, and is mainly used for rubber adhesives, synthetic resins, dyes, preservatives, medicines, analytical reagents and the like.
The technology for preparing the benzenediol by the hydroxylation reaction of the phenol and the hydrogen peroxide starts to be researched and developed from the late sixties of the last century in China and is industrially produced at present. However, with the continuous development of catalysts, the composition and the proportional components of reaction liquid are changed, and with the continuous development of high-end products in the downstream market of benzenediol, the quality requirement on intermediate benzenediol is more and more strict, and the existing market benzenediol products cannot meet the requirements of high-end customers.
In order to solve the above technical problems, the prior art has conducted many researches: for example, patent CN100344594C, CN101830780a of tianjin university discloses a separation and purification system and a purification method for phenol, catechol/hydroquinone and tar water solution, and the separation sequence is dehydration, dephenolization, decoking, catechol product rectification and hydroquinone product rectification separation. Compared with CN100344594C, CN101830780A optimizes energy saving and consumption reduction, and improves the purity of hydroquinone product: in the aspect of energy saving, if the first dephenolizing tower adopts normal pressure operation, the tower top adopts an internally returned condenser to produce the byproduct steam; the gas phase pipe at the top of the decoking distillation tower is directly connected with the catechol tower; in the aspect of product purification, for example, a hydroquinone refining tower is added, and a hydroquinone finished product is extracted from the upper side line of the tower.
Shanghai patent No. CN101054340A of Hua Yi acrylic acid Limited also discloses a separation and purification method of phenol and hydrogen peroxide reaction liquid, which comprises water, phenol, o/hydroquinone and tar, wherein the separation sequence comprises dehydration, phenol-water extraction, dephenolization, decoking and o/hydroquinone product rectification.
3238 Zxft 3238 chemical company CN 3262 Zxft 3262A discloses a method and apparatus for separating and purifying raw materials containing hydroquinone, resorcinol and possibly tar or catechol, firstly, a rectifying tower or a wiped film evaporator is adopted for continuous decoking, the decoked product is rectified by a catechol tower to obtain a finished catechol product, the bottom material of the catechol tower enters a product coarse distillation tower, resorcinol is extracted from the upper part of the coarse distillation tower to be melted and crystallized to obtain a finished resorcinol product, the bottom material of the coarse distillation tower enters a hydroquinone refining tower, and hydroquinone is extracted from the upper part of the refining tower to be melted and crystallized to obtain a finished hydroquinone product.
However, these techniques still have certain drawbacks: the technology is used for purifying two-component catechol and hydroquinone products; although the latter patent of Tianjin university optimizes energy conservation and consumption reduction and the purity of hydroquinone product, the latter patent still has the defects of over-high energy consumption and incapability of meeting the requirements of high-end customers in the market on the quality of catechol product, and simultaneously has the problems of tar puffing, coking, carbonization and the like in the process of extracting the product in the tar by adopting a deep steaming kettle, so that the material cannot flow normally;
in Shanghai Hua Yi acrylic acid Limited, tar is separated in the last step, and due to the fact that the tar is easy to swell, carbonize and crack after long retention time, normal production cannot be achieved, and the product purity is polluted;
luo Diya chemical company patent adopts a wiped film evaporator in the aspect of tar extraction to reduce the heat sensitivity of the product, but does not have further treatment, the content of hydroquinone in the tar is high, the rectified product is not further refined, and the quality of the hydroquinone product cannot meet the requirements of high-end customers in the market; in addition, the patent adopts a melt crystallizer to obtain resorcinol and hydroquinone, and has high operation difficulty and higher requirement on public works.
SUMMERY OF THE UTILITY MODEL
The utility model discloses go on to prior art defect and market demand, improve prior art, provide a benzenediol separation and purification system and method that phenol, hydrogen peroxide solution reaction were prepared to reduce the product energy consumption in hope, satisfy the high most advanced customer requirement in market simultaneously, also guarantee easy and simple to handle and production stability.
The utility model relates to a mixed liquid composition of phenol and hydrogen peroxide reaction is water, phenol, pyrocatechol, hydroquinone, resorcinol, tar, and the separation and purification method mainly contains the following steps:
(1) And (3) dehydrating: rectifying the reaction mixed liquid by a phenol dehydration tower, distilling phenol-containing water from the tower top, removing phenol water, and feeding the tower bottom into a phenol removal tower;
(2) And (3) phenol removal: rectifying the dehydrated/phenol tower bottoms by a dephenolizing tower, distilling off phenol at the tower top and returning to the reaction process, and removing the tower bottoms to a scraper evaporator;
(3) And (3) evaporation: evaporating the bottom from the dephenolizing tower by a scraper evaporator, allowing the upper part of the scraper evaporator to enter a phenol mixing tower in a gas phase state, discharging tar at the bottom, allowing the tar to enter a double-helix tar carbonizing machine, and further deeply evaporating;
(4) Decoking: rectifying the mixed phenol evaporated by a scraper evaporator and a double helix tar carbonizer by a phenol mixing tower, returning the distillate at the top to a dephenolizing tower, distilling crude catechol at the side line to a catechol refining tower, and feeding the material at the bottom to a hydroquinone refining tower;
(5) And (3) catechol refining: refining crude catechol from a lateral line of a phenol mixing tower by a catechol refining tower, returning light components at the top to the phenol mixing tower, distilling out catechol from the lateral line to a finished product receiving tank, and returning materials at the bottom to the phenol mixing tower;
(6) Refining hydroquinone: rectifying the materials from the bottom of the phenol mixing tower by a hydroquinone refining tower, distilling the materials from the top of the phenol mixing tower to obtain resorcinol-rich materials, removing the resorcinol-rich materials from the top of the phenol mixing tower, distilling the hydroquinone from the side of the phenol mixing tower to obtain a finished product receiving tank, and returning the bottoms of the phenol mixing tower to a scraper evaporator;
(7) Refining resorcinol: and distilling out light components from the top of the resorcinol rectifying tower to return to the phenol mixing tower, distilling out resorcinol from a side line to a finished product receiving tank, and returning the material at the bottom to the hydroquinone refining tower.
In order to realize the purpose, the utility model discloses specifically adopt following technical scheme:
the utility model provides a benzenediol separation and purification system that phenol, hydrogen peroxide solution reaction were prepared, including the dehydration phenol tower, dephenolization tower and the phenol tower that mixes that establish ties and set up, wherein dephenolization tower bottom in proper order is connected with scraper evaporator and spiral tar carbonization machine.
The top parts of the scraper evaporator and the spiral tar carbonizing machine are connected with a phenol mixing tower; the top of the phenol mixing tower is connected with a catechol refining tower, and the bottom of the phenol mixing tower is connected with a hydroquinone refining tower; the top of the hydroquinone refining tower is connected with the resorcinol refining tower, and the bottom of the hydroquinone refining tower is connected with the scraper evaporator; the top of the resorcinol refining tower and the bottom of the catechol refining tower are respectively connected with the phenol mixing tower.
Preferably, in the separation and purification system provided by the utility model, the rectification section of the dehydration phenol tower adopts tetrafluoro corrugated packing, the stripping section adopts metal plate corrugated packing, the tower top condenser adopts an internal reflux graphite condenser, and the rectification section and the tower internals adopt titanium alloy materials; the rectification section of the dephenolizing tower adopts wire mesh packing, the stripping section adopts metal plate corrugated packing, and the tower top condenser adopts an internal reflux graphite condenser; the rectification section and the stripping section of the phenol mixing tower adopt metal plate corrugated packing, and the tower top condenser is an internal reflux stainless steel condenser; the scraper evaporator and the double helix tar carbonizer are series-connected equipment for processing high-viscosity and heat-sensitive stainless steel materials; the rectification section and the stripping section of the catechol refining tower both adopt metal wire mesh packing, and the tower top condenser is an internal reflux stainless steel condenser; the rectification section and the stripping section of the hydroquinone refining tower are both made of metal plate corrugated packing, and a forced circulation pump is added at the bottom of the rectification tower; the rectifying section and the stripping section of the resorcinol refining tower both adopt metal wire mesh packing.
Preferably, in the separation and purification system provided by the utility model, the forced circulation pump is a high temperature magnetic gear pump which is high temperature resistant and viscous resistant.
Preferably, in the separation and purification system provided by the utility model, a distillate pipeline at the bottom of the dephenolizing tower is connected with a feeding pipe of the dephenolizing tower, a distillate pipeline at the top is connected with a dephenolizing water treatment process, and a distillate pipeline at the side part is connected with a water-containing phenol storage tank;
a distillate pipeline at the top of the dephenolizing tower is connected with a pure phenol storage tank, and a distillate pipeline at the bottom of the dephenolizing tower is connected with a scraper evaporator;
the top distillate pipeline of the phenol mixing tower is connected with the dephenolizing tower, the side distillate pipeline is connected with the catechol refining tower, and the bottom of the phenol mixing tower is connected with the hydroquinone refining tower;
the upper distillate pipeline of catechol refining is connected with a finished catechol receiving tank, and the bottom of the tower is connected with a phenol mixing tower;
the upper part of the hydroquinone refining tower is connected with the resorcinol refining tower, the side part of the hydroquinone refining tower is connected with a finished product hydroquinone receiving tank, and the tower bottom liquid is connected with a scraper evaporator;
the upper part of the resorcinol refining is connected with a phenol mixing tower through a distillation pipeline, a side line distillation pipeline is connected with a finished resorcinol receiving tank, and the bottom of the tower is connected with a hydroquinone refining tower.
Action and effect of the utility model
Compared with the prior art, the utility model provides a diphenol separation and purification system and method that phenol, hydrogen peroxide solution reaction were prepared not only greatly reduced product energy consumption satisfies the high most advanced customer requirement in market simultaneously, also guarantees easy and simple to handle and production stability, specifically expounds as follows:
the dehydration phenol tower is used for dehydration and dephenolization, and the phenol containing part of water is removed to be used for a reaction formula, so that the problems of long process route, low yield, high energy consumption, high investment cost and the like caused by completely removing water in the phenol in other patents are solved; the dehydration/phenol tower condenser is made of graphite materials, so that the problem that phenol water corrodes equipment is avoided, and the rectification section packing adopts tetrafluoro corrugated packing, so that the defects that the phenol water corrodes metal packing and ceramic packing are too high in specific gravity and are fragile and the like are avoided;
the dephenolizing tower adopts the reaction liquid as the cold medium of the condenser, so that the energy consumption is greatly saved;
the utility model discloses mix phenol column top and distill the side line and withdraw phenol, avoid because of dephenolization tower does not take off totally or because of tar schizolysis output phenol pollutes pyrocatechol product, pyrocatechol refining tower solves because of the oxidation or other components that the rectification schizolysis produced influence pyrocatechol colour quality and other indexes, provides outstanding quality for high-end customer; the bottom of the hydroquinone refining tower adopts a high-temperature magnetic gear pump for forced circulation, thereby avoiding the influence on the evaporation effect due to the large viscosity of materials in a tower kettle, and simultaneously avoiding the vacuum breaking in the tower and the difficult conveying of high-viscosity materials caused by the leakage of a pump in the rectifying tower;
the utility model adopts the hydroquinone rectifying tower to crudely distill the resorcinol and combine the resorcinol rectifying tower to purify the resorcinol, which is easier to operate and control than the melt crystallization, has less accessory equipment and does not need the refrigerant of the harsh condition required by the melt crystallization;
the utility model discloses a scraper evaporator combines the purification product and draws hydroquinone in the tar with double helix tar carbonizing machine, has avoided the problem such as hydroquinone content height in tar heat sensitivity, the popped coking and the tar, with scraper evaporator and the direct next rectifying column that advances of double helix tar carbonizing machine evaporation gas phase, practiced thrift the energy and reduced equipment cost input.
Drawings
FIG. 1 is a schematic diagram of the process for separating and purifying dihydroxybenzene prepared by the reaction of phenol and hydrogen peroxide in the embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments and drawings. The following examples should not be construed, however, as limiting the scope of the invention.
The system for separating and purifying dihydroxybenzene prepared by reacting phenol and hydrogen peroxide provided by the embodiment is shown in fig. 1, and comprises a phenol dehydration tower 1, a phenol dehydration tower 2 and a phenol mixing tower 3 which are connected in series, wherein a scraper evaporator 4 and a spiral tar carbonizing machine 5 are sequentially connected to the bottom of the phenol dehydration tower.
The top parts of the scraper evaporator 4 and the spiral tar carbonizing machine 5 are connected with the phenol mixing tower 3; the top of the phenol mixing tower 3 is connected with a catechol refining tower 6, and the bottom is connected with a hydroquinone refining tower 7; the top 7 of the hydroquinone refining tower is connected with a resorcinol refining tower 8, and the bottom is connected with a scraper evaporator; the top of the resorcinol refining tower 8 and the bottom of the catechol refining tower 6 are respectively connected with the phenol mixing tower 4.
In the specific arrangement aspect, a rectification section of the dehydrated phenol tower 1 adopts tetrafluoro corrugated packing, a stripping section adopts metal plate corrugated packing, a tower top condenser adopts an internal reflux graphite condenser, and the rectification section and tower internals adopt titanium alloy materials; the rectification section of the dephenolizing tower 2 adopts wire mesh packing, the stripping section adopts metal plate corrugated packing, and the tower top condenser adopts an internal reflux graphite condenser; the rectification section and the stripping section of the phenol mixing tower 3 both adopt metal plate corrugated packing, and the tower top condenser is an internal reflux stainless steel condenser; the scraper evaporator 4 and the double helix tar carbonizer 5 are series-connected equipment for processing high-viscosity and heat-sensitive stainless steel materials; the rectification section and the stripping section of the catechol refining tower 6 both adopt metal wire mesh packing, and the tower top condenser is an internal reflux stainless steel condenser; the rectifying section and the stripping section of the hydroquinone rectifying tower 7 both adopt metal plate corrugated packing, and a forced circulation pump 9 (preferably a high-temperature resistant and viscous resistant high-temperature magnetic gear pump) is added at the bottom of the rectifying tower; the rectifying section and the stripping section of the resorcinol refining tower 8 both adopt wire mesh packing.
The distillate pipeline at the bottom of the dephenolizing tower 1 is connected with a feeding pipe of the dephenolizing tower 2, the distillate pipeline at the top is connected with a dephenolizing water treatment process, and the distillate pipeline at the side part is connected with a water-containing phenol storage tank; a distillate pipeline at the top of the dephenolizing tower 2 is connected with a pure phenol storage tank, and a distillate pipeline at the bottom is connected with a scraper evaporator 4; a distillate pipeline at the top of the phenol mixing tower 3 is connected with the dephenolizing tower 2, a side distillate pipeline is connected with the catechol refining tower 6, and the bottom of the phenol mixing tower 3 is connected with the hydroquinone refining tower 7; the distillate pipeline at the upper part of the catechol refining tower 6 is connected with a finished catechol receiving tank, and the tower bottom is connected with a phenol mixing tower 3; the upper part of a hydroquinone refining tower 7 is connected with a resorcinol refining tower 8, the side part of the hydroquinone refining tower is connected with a finished product hydroquinone receiving tank, and the tower bottom liquid is connected with a scraper evaporator 4; the upper part of the resorcinol refining tower 8 is connected with a phenol mixing tower through a distillation pipeline, a side line distillation pipeline is connected with a finished resorcinol receiving tank, and the bottom of the tower is connected with a hydroquinone refining tower 7.
The following describes specific application examples of the above separation and purification system:
specific application example 1
The composition was 60% phenol, 30% water, 5.5% catechol, 3.9% hydroquinone, 0.2% resorcinol, 0.4% tar feed solution.
(1) Dehydration and dephenolization
Feeding the raw material solution into a dehydration phenol tower at the flow rate of 200Kg/h under the operating conditions of the pressure of 30-40Kpa and the pressure difference of 2-4Kpa, the temperature in the tower of 140-160 ℃ and the reflux ratio of 1.0-2.0; 7.8 percent of phenol-containing water is extracted from the tower top and sent to the next procedure, phenol with 15 to 20 percent of water is extracted from the side line and returned to a phenol storage tank, and tower bottom liquid is sent to a dephenolizing tower at the flow rate of 28 Kg/h.
(2) Dephenolation
The operating conditions of the dephenolizing tower are that the pressure is 4-8Kpa and the differential pressure is 2-4Kpa, the temperature in the tower is 140-180 ℃, and the reflux ratio is 1.5-2.5; phenol with the phenol content more than or equal to 98.5 percent is extracted from the upper part of the dephenolizing tower, and the phenol is sent to a scraper evaporator at the bottom of the dephenolizing tower at the speed of 20 Kg/h.
(3) Evaporation and decoking
The gas phase at the top of the scraper evaporator enters a phenol mixing tower, tar containing 7-10% of hydroquinone at the bottom is discharged to a double-helix tar carbonizing machine for further evaporation, the operating conditions of the scraper evaporator are that the pressure is 2-4Kpa and the temperature is 170-220 ℃, and the operating conditions of the double-helix tar carbonizing machine are that the pressure is 2-4Kpa and the temperature is 220-240 ℃; the gas phase at the top of the scraper evaporator and the double helix tar carbonizer enters a phenol mixing tower at the flow rate of 19.2 Kg/h.
(4) Catechol purification
The upper part of the phenol mixing tower is extracted and returned to the phenol tower, pyrocatechol with the side line distillation rate of more than or equal to 99 percent is sent into a pyrocatechol refining tower at the flow rate of 10.5Kg/h, the operation conditions of the phenol mixing tower are that the pressure is 2-4Kpa and the pressure difference is 2-4Kpa, the temperature in the tower is 170-210 ℃, and the reflux ratio is 1.5-2.5; the finished catechol with the content of more than or equal to 99.9 percent is extracted from the top of the catechol refining tower, and enters a catechol receiving tank at the flow rate of 10.3Kg/h, and the bottom of the catechol refining tower is intermittently mixed with the phenol tower under the operating conditions of the pressure of 2-3Kpa and the pressure difference of 2-4Kpa, the temperature in the tower is 170-210 ℃, and the reflux ratio is 1.0-1.5.
(5) Hydroquinone refining
Feeding the phenol mixing tower kettle into a hydroquinone refining tower at the flow rate of 8.2Kg/h, feeding resorcinol with the distillate content of more than or equal to 90 percent at the upper part of the hydroquinone refining tower into the resorcinol refining tower, feeding a side-draw finished product hydroquinone with the distillate content of more than or equal to 99.5 percent into a hydroquinone receiving tank at the flow rate of 7.3Kg/h, and feeding the residue liquid back to a scraper evaporator, wherein the operating conditions of the hydroquinone tower are that the pressure is 2-4Kpa and the pressure difference is 2-4Kpa, the temperature in the hydroquinone tower is 190-240 ℃, and the reflux ratio is 2.0-3.0;
(6) Purification of resorcinol
The upper distillate of resorcinol refining is returned to the phenol mixing tower, the content of the side distillate is more than or equal to 99.5 percent of finished resorcinol, the finished resorcinol is sent to a resorcinol receiving tank at a rate of 0.37Kg/h, and the tower bottom liquid is returned to the hydroquinone refining tower; the operation conditions of the resorcinol tower are that the pressure is 2-3Kpa, the pressure difference is 2-4Kpa, the temperature in the tower is 170-220 ℃, and the reflux ratio is 2.0-3.0.
Concrete application example 2
The composition was 39% phenol, 50% water, 3.0% catechol, 7.0% hydroquinone, 0.3% resorcinol, 0.7% tar feed solution.
(1) Dewatering and dephenolizing
Feeding into a dehydration/phenol tower at a flow rate of 200Kg/h, wherein the operation conditions of the dehydration/phenol tower are that the pressure is 30-40Kpa, the pressure difference is 2-4Kpa, the temperature in the tower is 140-160 ℃, and the reflux ratio is 1.0-2.0; 7.8 percent of phenol-containing water is extracted from the tower top and sent to the next procedure, phenol with 15 to 20 percent of water is extracted from the side line and returned to a phenol storage tank, and tower bottom liquid is sent to a dephenolizing tower at the flow rate of 26 Kg/h;
(2) Dephenolation
The operating conditions of the dephenolizing tower are that the pressure is 4-8Kpa and the differential pressure is 2-4Kpa, the temperature in the tower is 140-180 ℃, and the reflux ratio is 1.5-2.5; phenol with the phenol content more than or equal to 98.5 percent is extracted from the upper part of the dephenolizing tower, and the phenol is sent into a scraper evaporator at the bottom of the dephenolizing tower at a rate of 22 Kg/h;
(3) Evaporation and decoking
The gas phase at the top of the scraper evaporator enters a phenol mixing tower, tar containing 7-10% of hydroquinone at the bottom is discharged to a double-helix tar carbonizing machine for further evaporation, the operating conditions of the scraper evaporator are 2-4Kpa of pressure and 170-220 ℃, and the operating conditions of the double-helix tar carbonizing machine are 2-4Kpa of pressure and 220-240 ℃;
(4) Catechol purification
The gas phase at the top of the scraper evaporator and the double helix tar carbonizer enters a phenol mixing tower at the flow rate of 20.4Kg/h, the upper part of the phenol mixing tower is extracted to return to the phenol tower, pyrocatechol with the side line distillate of more than or equal to 99 percent is sent to a pyrocatechol refining tower at the flow rate of 5.7Kg/h, the operation conditions of the phenol mixing tower are 2-4Kpa and 2-4Kpa of differential pressure, the temperature in the tower is 170-210 ℃, and the reflux ratio is 1.5-2.5; the method comprises the following steps of (1) extracting finished catechol with the content of more than or equal to 99.9 percent from the top of a catechol refining tower, feeding the finished catechol into a catechol receiving tank at the flow rate of 5.6Kg/h, and returning the finished catechol to a phenol tower from the bottom of the catechol refining tower at the gap, wherein the operation conditions are that the pressure is 2-3Kpa and the pressure difference is 2-4Kpa, the temperature in the tower is 170-210 ℃, and the reflux ratio is 1.0-1.5;
(5) Hydroquinone refining
Feeding the phenol mixing tower kettle into a hydroquinone refining tower at a flow rate of 14.6Kg/h, feeding resorcinol with a distillate content of more than or equal to 90 percent at the upper part of the hydroquinone refining tower into the resorcinol refining tower, feeding a side-draw finished product hydroquinone with a side-draw content of more than or equal to 99.5 percent into a hydroquinone receiving tank at 13.6Kg/h, and feeding the residue liquid back to a scraper evaporator, wherein the operating conditions of the hydroquinone tower are that the pressure is 2-4Kpa and the pressure difference is 2-4Kpa, the temperature in the hydroquinone tower is 190-240 ℃, and the reflux ratio is 2.0-3.0;
(6) Purification of resorcinol
The upper distillate of resorcinol refining is returned to the phenol column, the content of the distillate at the side line is more than or equal to 99.5 percent of resorcinol finished product, the distillate is sent to a resorcinol receiving tank at the rate of 0.54Kg/h, and the bottom liquid of the column is returned to the hydroquinone refining column; the operation conditions of the resorcinol tower are that the pressure is 2-3Kpa, the pressure difference is 2-4Kpa, the temperature in the tower is 170-220 ℃, and the reflux ratio is 2.0-3.0.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above embodiments, and that the foregoing embodiments and descriptions are provided only to illustrate the principles of the present invention without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A system for separating and purifying benzenediol prepared by reacting phenol and hydrogen peroxide is characterized by comprising a phenol dehydrating tower, a phenol dehydrating tower and a phenol mixing tower which are connected in series; the bottom of the dephenolizing tower is sequentially connected with a scraper evaporator and a spiral tar carbonizing machine, and the tops of the scraper evaporator and the spiral tar carbonizing machine are connected with the phenol mixing tower; the top of the phenol mixing tower is connected with a catechol refining tower, and the bottom of the phenol mixing tower is connected with a hydroquinone refining tower; the top of the hydroquinone refining tower is connected with the resorcinol refining tower, the bottom of the hydroquinone refining tower is connected with the scraper evaporator,
the top of the resorcinol refining tower and the bottom of the catechol refining tower are respectively connected with the phenol mixing tower.
2. The separation and purification system of claim 1, wherein:
wherein, the rectification section of the dehydrated phenol tower adopts tetrafluoro corrugated packing, the stripping section adopts metal plate corrugated packing, the tower top condenser adopts an internal reflux graphite condenser, and the rectification section and the tower internals adopt titanium alloy materials;
the rectification section of the dephenolizing tower adopts wire mesh packing, the stripping section adopts metal plate corrugated packing, and the tower top condenser adopts an internal reflux graphite condenser;
the rectification section and the stripping section of the phenol mixing tower adopt metal plate corrugated packing, and the tower top condenser is an internal reflux stainless steel condenser;
the scraper evaporator and the double helix tar carbonizer are series-connected equipment for processing high-viscosity and heat-sensitive stainless steel materials;
the rectification section and the stripping section of the catechol refining tower both adopt metal wire mesh packing, and the tower top condenser is an internal reflux stainless steel condenser;
the rectifying section and the stripping section of the hydroquinone rectifying tower both adopt metal plate corrugated packing, and a forced circulation pump is added at the bottom of the rectifying tower;
and the rectifying section and the stripping section of the resorcinol refining tower both adopt wire mesh fillers.
3. The separation and purification system according to claim 2, wherein:
wherein, the forced circulation pump is a high-temperature magnetic gear pump with high temperature resistance and viscosity resistance.
4. The separation and purification system of claim 1, wherein:
the bottom distillate pipeline of the dehydration phenol tower is connected with a feeding pipe of the dehydration phenol tower, the top distillate pipeline is connected with a phenol removing water treatment process, and the side distillate pipeline is connected with a water-containing phenol storage tank;
the top distillate pipeline of the dephenolizing tower is connected with a pure phenol storage tank, and the bottom distillate pipeline is connected with a scraper evaporator;
a distillate pipeline at the top of the phenol mixing tower is connected with a dephenolizing tower, a side distillate pipeline is connected with a catechol refining tower, and the bottom of the phenol mixing tower is connected with a hydroquinone refining tower;
the distillate pipeline at the upper part of the catechol refining tower is connected with a finished catechol receiving tank, and the bottom of the catechol refining tower is connected with a phenol mixing tower;
the upper part of the hydroquinone refining tower is connected with the resorcinol refining tower, the side part of the hydroquinone refining tower is connected with a finished product hydroquinone receiving tank, and the tower bottom liquid is connected with a scraper evaporator;
the upper part of the resorcinol refining tower is connected with a phenol mixing tower through a distillation pipeline, a side line distillation pipeline is connected with a finished resorcinol receiving tank, and the bottom of the resorcinol refining tower is connected with a hydroquinone refining tower.
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