CN110577462A - method and device for recovering ditrimethylolpropane - Google Patents
method and device for recovering ditrimethylolpropane Download PDFInfo
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- CN110577462A CN110577462A CN201910953680.1A CN201910953680A CN110577462A CN 110577462 A CN110577462 A CN 110577462A CN 201910953680 A CN201910953680 A CN 201910953680A CN 110577462 A CN110577462 A CN 110577462A
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- 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
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- 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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- 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
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/44—Separation; Purification; Stabilisation; Use of additives by treatments giving rise to a chemical modification
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- C07D319/04—1,3-Dioxanes; Hydrogenated 1,3-dioxanes
- C07D319/06—1,3-Dioxanes; Hydrogenated 1,3-dioxanes not condensed with other rings
Abstract
The invention discloses a method and a device for recovering ditrimethylolpropane, wherein the method for recovering ditrimethylolpropane comprises the following steps of S1: acidifying the raw materials to obtain a mixed material; s2: performing primary rectification treatment on the mixed material to obtain a primary rectification product, wherein the primary rectification product comprises a mixed fraction containing CTF, TMP and DTMP and light components of CTF and TMP; s3: and carrying out secondary rectification treatment on the mixed fraction to obtain a secondary rectification product, wherein the secondary rectification product comprises a DTMP crude product containing DTMP and light components CTF and TMP. The ditrimethylolpropane recovery device comprises an acidification kettle, a primary rectifying device and a secondary rectifying device, wherein the primary rectifying device is connected with an outlet of the acidification kettle; and the secondary rectifying device is connected with the primary rectifying device. The invention can improve the yield of the DTMP, further improve the yield of the DTMP, simultaneously obtain TMP and CTF and improve the economic benefit.
Description
Technical Field
The invention relates to a method and a device for recovering ditrimethylolpropane.
background
a trimethylolpropane apparatus (hereinafter referred to as a TMP apparatus) is an apparatus for producing trimethylolpropane (hereinafter referred to as TMP). At present, ditrimethylolpropane (hereinafter referred to as DTMP) is produced by mainly adopting a crystallization separation method or adopting a crystallization separation method after purification for heavy components remained in a TMP device, and the DTMP has special performance and wide application in electronic chemicals, especially UV light-cured resin. However, the heavy components remaining in the TMP device contain impurities such as TMP and derivatives thereof, so that the yield of the DTMP is less than 50%, which seriously affects the yield of the DTMP, and the DTMP is in a state of short supply throughout the year.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide a method for recovering ditrimethylolpropane, which can improve the yield of DTMP, further improve the yield of the DTMP, simultaneously obtain TMP and trimethylolpropane cyclic formal (hereinafter referred to as CTF) and improve economic benefits.
in order to solve the technical problems, the technical scheme of the invention is as follows: a method for recovering ditrimethylolpropane comprises the following steps:
s1: acidifying raw materials to obtain a mixed material, wherein the raw materials are derived from heavy components remained in a TMP device or residues obtained after DTMP is extracted from the heavy components remained in the TMP device through a crystallization separation method;
s2: carrying out primary rectification treatment on the mixed material to obtain a primary rectification product by separation, wherein the primary rectification product comprises a mixed fraction containing CTF, TMP and DTMP and light components of CTF and TMP;
S3: and carrying out secondary rectification treatment on the mixed fraction to separate and obtain a secondary rectification product, wherein the secondary rectification product comprises a DTMP crude product containing DTMP and light components CTF and TMP.
further, in step S1, the step of the acidification processing is as follows:
the raw materials are mixed with a proper amount of water and a proper amount of acid and stirred.
Further, the acid is solid acid, and/or the temperature of the acidification treatment is 155 ℃ and ~ 165 ℃, and/or the time of the acidification treatment is 2 ~ 3 hours.
further, the acidification treatment and/or the primary rectification treatment and/or the secondary rectification treatment are/is carried out in a negative pressure environment.
the invention also provides a ditrimethylolpropane recovery device, which comprises:
acidifying the kettle;
the primary rectifying device is connected with an outlet of the acidification kettle;
The secondary rectifying device is connected with the primary rectifying device; wherein the content of the first and second substances,
the acidification kettle is used for at least accessing raw materials and acid so as to carry out acidification treatment on the raw materials to obtain a mixed material; the raw material is derived from residual heavy components in a TMP device or residues obtained after DTMP is extracted from the residual heavy components in the TMP device by a crystallization separation method;
The primary rectification device is used for carrying out primary rectification treatment on the mixed material obtained after the acidification treatment of the acidification kettle so as to separate and obtain a primary rectification product; the first-stage rectification product comprises a mixed fraction containing CTF, TMP and DTMP and light components of CTF and TMP;
the secondary rectification device is used for carrying out secondary rectification treatment on the mixed fraction obtained after the primary rectification treatment of the primary rectification device so as to separate and obtain a secondary rectification product; the secondary rectification product comprises a DTMP crude product containing DTMP and light components CTF and TMP.
Further provides a concrete structure of the primary rectifying device, the primary rectifying device comprises a first rectifying tower, a first circulating pump, a first reboiler, a first condenser, a first reflux container and a first reflux pump, wherein,
An outlet of the acidification kettle is connected with a material inlet of the first rectifying tower, so that the mixed material flows into the first rectifying tower;
the second-stage rectifying device is connected with a middle fraction outlet of the first rectifying tower, so that the mixed fraction in the first rectifying tower flows into the second-stage rectifying device;
an inlet of the first circulating pump is connected with a heavy component outlet of the first rectifying tower;
the outlet of the first circulating pump is connected with the inlet of the first reboiler;
The outlet of the first reboiler is connected with the light component inlet of the first rectifying tower;
an inlet of the first condenser is connected with a light component outlet of the first rectifying tower, so that the light components CTF and TMP rectified and separated by the first rectifying tower flow into the first condenser to be condensed and liquefied;
the inlet of the first reflux vessel is connected with the outlet of the first condenser, so that the liquefied CTF and TMP condensed by the first condenser flow into the first reflux vessel for storage;
and the inlet of the first reflux pump is connected with the outlet of the first reflux container, and the outlet of the first reflux pump is connected with the reflux inlet of the first rectifying tower.
further provides a specific structure of the secondary rectification device, the secondary rectification device comprises a second rectification tower, a second circulating pump, a second reboiler, a second condenser, a second reflux container and a second reflux pump, wherein,
A fraction inlet of the second rectifying tower is connected with the primary rectifying device so that the mixed fraction flows into the second rectifying tower;
An inlet of the second circulating pump is connected with a heavy component outlet of the second rectifying tower;
the outlet of the second circulating pump is connected with the inlet of the second reboiler;
the outlet of the second reboiler is connected with the light component inlet of the second rectifying tower;
An inlet of the second condenser is connected with a light component outlet of the second rectifying tower, so that the light components CTF and TMP rectified and separated by the second rectifying tower flow into the second condenser to be condensed and liquefied;
The inlet of the second reflux container is connected with the outlet of the second condenser, so that the liquefied CTF and TMP condensed by the second condenser flow into the second reflux container to be stored;
and the inlet of the second reflux pump is connected with the outlet of the second reflux container, and the outlet of the second reflux pump is connected with the reflux inlet of the second rectifying tower.
Further, the apparatus for recovering ditrimethylolpropane further comprises:
the raw material pump is connected between the acidification kettle and the primary rectifying device so as to pump the mixture in the acidification kettle into the primary rectifying device;
The heating device is connected between the acidification kettle and the primary rectifying device and is used for heating the mixed material flowing into the primary rectifying device from the acidification kettle;
And/or a third circulating pump, wherein an inlet of the third circulating pump is connected with a circulating outlet of the acidification kettle, and an outlet of the third circulating pump is connected with a circulating inlet of the acidification kettle, so that the mixed material circularly flows in the acidification kettle.
Further, the ditrimethylolpropane recovery device also comprises a vacuumizing device, and the vacuumizing device is connected with the acidification kettle and/or the primary rectification device and/or the secondary rectification device, so that the vacuumizing device can vacuumize the acidification kettle and/or the primary rectification device and/or the secondary rectification device.
further, the vacuumizing device is connected with the acidification kettle and/or the primary rectifying device and/or the secondary rectifying device through a tail gas cooler.
after the technical scheme is adopted, the raw materials, a proper amount of water and a proper amount of acid are placed into the acidification kettle to be mixed, the raw materials are stirred by a stirring device to accelerate the acidification treatment of the raw materials, and a mixed material is obtained; the raw material pump pumps the mixture into the first rectifying tower, the first rectifying tower carries out primary rectifying treatment on the mixture so as to obtain a mixed fraction containing CTF, TMP and DTMP and light components of CTF and TMP through rectification, and the light components of CTF and TMP in the first rectifying tower flow into the first condenser for condensation and liquefaction and then flow into the first reflux container for storage; and the mixed fraction in the first rectifying tower flows into the second rectifying tower, the second rectifying tower carries out secondary rectification treatment on the mixed fraction so as to obtain a DTMP crude product containing DTMP and light components CTF and TMP through rectification, the light components CTF and TMP in the second rectifying tower flow into the second condenser for condensation and liquefaction, and then flow into the second reflux container for storage, and the residual fraction in the second rectifying tower is the DTMP crude product. The method not only improves the yield and the yield of the DTMP, but also improves the yield of the DTMP from 50% to 90%, and simultaneously can extract the CTF and the TMP, thereby improving the economic benefit of enterprises and reducing the waste of raw materials.
drawings
FIG. 1 is a schematic view of a structure of a ditrimethylolpropane recovery apparatus of the present invention;
FIG. 2 is a schematic diagram of the structure of the acidification kettle of the invention.
Detailed Description
in order that the present invention may be more readily and clearly understood, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments that are illustrated in the appended drawings.
example one
a method for recovering ditrimethylolpropane comprises the following steps:
S1: acidifying raw materials to obtain a mixed material, wherein the raw materials are derived from heavy components remained in a TMP device or residues obtained after DTMP is extracted from the heavy components remained in the TMP device through a crystallization separation method;
s2: carrying out primary rectification treatment on the mixed material to obtain a primary rectification product by separation, wherein the primary rectification product comprises a mixed fraction containing CTF, TMP and DTMP and light components of CTF and TMP;
S3: and carrying out secondary rectification treatment on the mixed fraction to separate and obtain a secondary rectification product, wherein the secondary rectification product comprises a DTMP crude product containing DTMP and light components CTF and TMP. In this embodiment, the raw material is derived from a residue obtained after extracting DTMP from a residual recombinant fraction in a TMP device by a crystallization separation method, the raw material contains TMP, DTMP and trimethylolpropane linear formal (hereinafter referred to as LMTMP), and the LMTMP can be converted into TMP and CTF by an acidification treatment, the method can also obtain CTF and TMP while recovering the TMP, and the CTF can be used as a raw material of high-grade grease or a UV light curing monomer, which is beneficial to improving the economic benefit of an enterprise and also improves the yield of the TMP; the primary rectification product also comprises kettle residues after primary rectification treatment, and the kettle residues can be used as raw materials for synthesizing polyester polyol after being mixed with a proper amount of CTF and TMP, so that material waste is reduced, and the utilization rate of the materials is improved; the crude DTMP product can be extracted by the existing methods such as a crystallization separation method and the like. Specifically, the TMP device is a device for producing TMP, and the specific structure thereof is the prior art well known to those skilled in the art, and is not described in detail in this embodiment; when the TMP device produces TMP, recombinant components remain in the TMP device; extracting DTMP from heavy components remaining in a TMP device by a crystallization separation method, or extracting and purifying DTMP and then extracting DTMP by a crystallization separation method is a conventional DTMP extraction method adopted by manufacturers in the field at present, and details are not described in this embodiment.
in step S1, the acidification process is as follows:
The raw materials are mixed and stirred with a proper amount of water and a proper amount of acid, specifically, the mass percent of the water during mixing can be 2% ~ 5%, and in the embodiment, the mass percent of the water during mixing is 5%.
specifically, the acid may be a solid acid, the PH of the solid acid may be 2.4 ~ 4.0.0, preferably 2.5, the solid acid may be a cation exchange resin of sulfonic acid supported on silica gel, or a cation exchange resin of benzenesulfonic acid supported on silica gel, or a cation exchange resin of toluenesulfonic acid supported on silica gel, the temperature of the acidification treatment may be 155 ℃ to ~ 165 ℃, and the time of the acidification treatment may be 2 ~ 3 hours, in this embodiment, the temperature of the acidification treatment is 160 ℃, and the time of the acidification treatment is 2.5 hours.
In this embodiment, the acidification treatment, the primary rectification treatment and the secondary rectification treatment may be performed in a negative pressure environment.
example two
As shown in fig. 1 and 2, a ditrimethylolpropane recovery device comprises:
acidifying the kettle 1;
the primary rectifying device is connected with an outlet of the acidification kettle 1;
the secondary rectifying device is connected with the primary rectifying device; wherein the content of the first and second substances,
the acidification kettle 1 is used for at least accessing raw materials and acid so as to carry out acidification treatment on the raw materials to obtain a mixed material; the raw material is derived from residual heavy components in a TMP device or residues obtained after DTMP is extracted from the residual heavy components in the TMP device by a crystallization separation method; in this example, the feedstock is derived from the residue of a TMP unit from which the residual recombinant fraction has been subjected to a crystallization separation process to extract DTMP;
the primary rectification device is used for carrying out primary rectification treatment on the mixed material obtained after the acidification treatment of the acidification kettle 1 so as to separate and obtain a primary rectification product; the first-stage rectification product comprises a mixed fraction containing CTF, TMP and DTMP and light components of CTF and TMP;
the secondary rectification device is used for carrying out secondary rectification treatment on the mixed fraction obtained after primary rectification treatment of the primary rectification device to obtain a secondary rectification product through separation, the secondary rectification product comprises a DTMP crude product containing DTMP and light components CTF and TMP, specifically, the acid can be solid acid, the pH value of the solid acid can be 2.4 ~ 4.0.0, preferably 2.5, the solid acid can be cation exchange resin of sulfonic acid loaded by silica gel, or cation exchange resin of benzene sulfonic acid loaded by silica gel, or cation exchange resin of methyl benzene sulfonic acid loaded by silica gel, the raw materials contain TMP, DTMP and LMTMP, and the LMTMP can be converted into TMP and CTF through acidification treatment.
As shown in fig. 1 and 2, the first-stage rectification apparatus is, for example, but not limited to, a structure including a first rectification column 2, a first circulation pump 3, a first reboiler 4, a first condenser 5, a first reflux vessel 6, and a first reflux pump 19, wherein,
the outlet of the acidification kettle 1 is connected with the material inlet of the first rectifying tower 2, so that the mixed material flows into the first rectifying tower 2;
The secondary rectification device is connected with a middle fraction outlet of the first rectification tower 2, so that the mixed fraction in the first rectification tower 2 flows into the secondary rectification device;
An inlet of the first circulating pump 3 is connected with a heavy component outlet of the first rectifying tower 2;
the outlet of the first circulation pump 3 is connected to the inlet of the first reboiler 4;
an outlet of the first reboiler 4 is connected to a light component inlet of the first rectification column 2;
an inlet of the first condenser 5 is connected with a light component outlet of the first rectifying tower 2, so that the light components CTF and TMP rectified and separated by the first rectifying tower 2 flow into the first condenser 5 to be condensed and liquefied;
An inlet of the first reflux vessel 6 is connected with an outlet of the first condenser 5, so that the liquefied CTF and TMP condensed by the first condenser 5 flows into the first reflux vessel 6 to be stored;
An inlet of the first reflux pump 19 is connected with an outlet of the first reflux container 6, and an outlet of the first reflux pump 19 is connected with a reflux inlet of the first rectifying tower 2, so that the separation accuracy of the CTF and the TMP in the first reflux container 6 is improved. Specifically, the first circulation pump 3 is configured to pump the mixture in the first rectification column 2 to the first reboiler 4 so as to rectify the mixture to obtain a mixed fraction containing CTF, TMP, and DTMP and light components CTF and TMP, and specific structures of the first rectification column 2, the first circulation pump 3, the first reboiler 4, and the first condenser 5 are all the prior art, and are not specifically described in detail in this embodiment.
As shown in fig. 1 and 2, the second rectification apparatus is, for example, but not limited to, a structure comprising a second rectification column 7, a second circulation pump 8, a second reboiler 9, a second condenser 10, a second reflux vessel 11 and a second reflux pump 20, wherein,
a fraction inlet of the second rectifying tower 7 is connected with the primary rectifying device, so that the mixed fraction flows into the second rectifying tower 7;
an inlet of the second circulating pump 8 is connected with a heavy component outlet of the second rectifying tower 7;
The outlet of the second circulating pump 8 is connected with the inlet of the second reboiler 9;
The outlet of the second reboiler 9 is connected with the light component inlet of the second rectifying tower 7;
an inlet of the second condenser 10 is connected with a light component outlet of the second rectifying tower 7, so that the light components CTF and TMP rectified and separated by the second rectifying tower 7 flow into the second condenser 10 to be condensed and liquefied;
An inlet of the second reflux vessel 11 is connected to an outlet of the second condenser 10, so that the liquefied CTF and TMP condensed by the second condenser 10 flows into the second reflux vessel 11 to be stored;
The inlet of the second reflux pump 20 is connected with the outlet of the second reflux container 11, and the outlet of the second reflux pump 20 is connected with the reflux inlet of the second rectifying tower 7, so as to improve the separation accuracy of the CTF and the TMP in the second reflux container 11. Specifically, the second circulation pump 8 is configured to pump the mixed fraction in the second rectification column 7 to the second reboiler 9, so as to rectify the mixed fraction to obtain a crude DTMP product containing DTMP and light components CTF and TMP, in this embodiment, the mass percentage of DTMP in the crude DTMP product is not less than 85%, the specific structures of the second rectification column 7, the second circulation pump 8, the second reboiler 9, and the second condenser 10 are all the prior art, and details are not described in this embodiment.
As shown in fig. 1 and 2, the apparatus for recovering ditrimethylolpropane may further include:
a raw material pump 12, wherein the raw material pump 12 is connected between the acidification kettle 1 and the primary rectification device so as to pump the mixture in the acidification kettle 1 into the primary rectification device;
The heating device 13 is connected between the acidification kettle 1 and the primary rectifying device, and is used for heating the mixed material flowing into the primary rectifying device from the acidification kettle 1; specifically, the acidification kettle 1 is connected with a first rectifying tower 2 in the primary rectifying device, and the raw material pump 12 and the heating device 13 are sequentially connected in series between the acidification kettle 1 and the first rectifying tower 2; in this embodiment, the temperature in the acidification kettle 1 is 160 ℃, the heating device 13 is used for heating the mixed material to 230 ℃, the heating device 13 may be a heat exchanger, the specific structure of the heat exchanger is the prior art, and details are not described in this embodiment.
as shown in fig. 1 and 2, the apparatus for recovering ditrimethylolpropane may further include:
An inlet of the third circulating pump 14 is connected with a circulating outlet of the acidification kettle 1, and an outlet of the third circulating pump 14 is connected with a circulating inlet of the acidification kettle 1, so that the mixed material circularly flows in the acidification kettle 1; in order to accelerate the acidification treatment in the acidification tank 1.
in this embodiment, the acidification kettle 1 includes a stirring device, the stirring device includes a power source 15 and a stirring rod 16, one end of the stirring rod 16 extends into the acidification kettle 1, and the other end of the stirring rod 16 is connected to the power source 15, so that the power source 15 drives the stirring rod 16 to rotate to stir the mixed material, so as to further accelerate the acidification treatment speed in the acidification kettle 1, in this embodiment, the power source 15 may be a motor.
as shown in fig. 1 and 2, the ditrimethylolpropane recovery device may further include a vacuum extractor 17, and the vacuum extractor 17 is connected to the acidification kettle 1, the first rectification device and the second rectification device, so that the vacuum extractor 17 can extract vacuum from the acidification kettle 1, the first rectification device and the second rectification device.
Specifically, the vacuumizing device 17 is connected with the acidification kettle 1, the primary rectifying device and the secondary rectifying device through a tail gas cooler 18; in this embodiment, the tail gas cooler 18 is connected to the acidification kettle 1, the first rectification tower 2 and the second rectification tower 7, respectively, so that the vacuumizing device 17 vacuumizes the acidification kettle 1, the first rectification tower 2 and the second rectification tower 7, and the specific structures of the vacuumizing device 17 and the tail gas cooler 18 are the prior art, which is not described in detail in this embodiment.
the working principle of the invention is as follows:
putting the raw materials, a proper amount of water and a proper amount of acid into the acidification kettle 1 for mixing, stirring by the stirring device to accelerate the acidification treatment of the raw materials, and obtaining a mixed material; the raw material pump 12 pumps the mixture into the first rectification tower 2, the first rectification tower 2 performs primary rectification treatment on the mixture so as to obtain a mixed fraction containing CTF, TMP and DTMP and light components CTF and TMP through rectification, the light components CTF and TMP in the first rectification tower 2 flow into the first condenser 5 for condensation and liquefaction and then flow into the first reflux container 6 for storage; the mixed fraction in the first rectifying tower 2 flows into the second rectifying tower 7, the second rectifying tower 7 performs secondary rectification treatment on the mixed fraction so as to obtain a DTMP crude product containing DTMP and light components CTF and TMP through rectification, the light components CTF and TMP in the second rectifying tower 7 flow into the second condenser 10 for condensation and liquefaction, and then flow into the second reflux container 11 for storage, and the residual fraction in the second rectifying tower 7 is the DTMP crude product. The method not only improves the yield and the yield of the DTMP, but also improves the yield of the DTMP from 50% to 90%, and simultaneously can extract the CTF and the TMP, thereby improving the economic benefit of enterprises and reducing the waste of raw materials.
The above embodiments are described in further detail to solve the technical problems, technical solutions and advantages of the present invention, and it should be understood that the above embodiments are only examples of the present invention and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
in the description of the present invention, it is to be understood that the terms indicating an orientation or positional relationship are based on the orientation or positional relationship shown in the drawings only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
in the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
in the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
furthermore, the terms "horizontal", "vertical", "overhang" and the like do not imply that the components are required to be absolutely horizontal or overhang, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the present invention, unless otherwise expressly stated or limited, the first feature may be present on or under the second feature in direct contact with the first and second feature, or may be present in the first and second feature not in direct contact but in contact with another feature between them. Also, the first feature being above, on or above the second feature includes the first feature being directly above and obliquely above the second feature, or merely means that the first feature is at a higher level than the second feature. A first feature that underlies, and underlies a second feature includes a first feature that is directly under and obliquely under a second feature, or simply means that the first feature is at a lesser level than the second feature.
Claims (10)
1. a method for recovering ditrimethylolpropane is characterized by comprising the following steps:
s1: acidifying raw materials to obtain a mixed material, wherein the raw materials are derived from heavy components remained in a TMP device or residues obtained after DTMP is extracted from the heavy components remained in the TMP device through a crystallization separation method;
s2: carrying out primary rectification treatment on the mixed material to obtain a primary rectification product by separation, wherein the primary rectification product comprises a mixed fraction containing CTF, TMP and DTMP and light components of CTF and TMP;
s3: and carrying out secondary rectification treatment on the mixed fraction to separate and obtain a secondary rectification product, wherein the secondary rectification product comprises a DTMP crude product containing DTMP and light components CTF and TMP.
2. the method for recovering ditrimethylolpropane according to claim 1, wherein in step S1, the acidification step is as follows:
the raw materials are mixed with a proper amount of water and a proper amount of acid and stirred.
3. the method of recovering ditrimethylolpropane according to claim 2, wherein,
the acid is solid acid, and/or the temperature of the acidification treatment is 155 ℃ and ~ 165 ℃, and/or the time of the acidification treatment is 2 ~ 3 h.
4. The method of recovering ditrimethylolpropane according to claim 1, wherein,
And the acidification treatment and/or the primary rectification treatment and/or the secondary rectification treatment are/is carried out in a negative pressure environment.
5. a ditrimethylolpropane recovery device is characterized by comprising:
An acidification kettle (1);
The primary rectifying device is connected with an outlet of the acidification kettle (1);
the secondary rectifying device is connected with the primary rectifying device; wherein the content of the first and second substances,
The acidification kettle (1) is used for at least accessing raw materials and acid so as to carry out acidification treatment on the raw materials to obtain a mixed material; the raw material is derived from residual heavy components in a TMP device or residues obtained after DTMP is extracted from the residual heavy components in the TMP device by a crystallization separation method;
the primary rectification device is used for carrying out primary rectification treatment on the mixed material obtained after the acidification treatment of the acidification kettle (1) so as to separate and obtain a primary rectification product; the first-stage rectification product comprises a mixed fraction containing CTF, TMP and DTMP and light components of CTF and TMP;
the secondary rectification device is used for carrying out secondary rectification treatment on the mixed fraction obtained after the primary rectification treatment of the primary rectification device so as to separate and obtain a secondary rectification product; the secondary rectification product comprises a DTMP crude product containing DTMP and light components CTF and TMP.
6. The apparatus for recovering ditrimethylolpropane according to claim 5,
The primary rectifying device comprises a first rectifying tower (2), a first circulating pump (3), a first reboiler (4), a first condenser (5), a first reflux container (6) and a first reflux pump (19), wherein,
the outlet of the acidification kettle (1) is connected with the material inlet of the first rectifying tower (2), so that the mixed material flows into the first rectifying tower (2);
The secondary rectification device is connected with a middle fraction outlet of the first rectification tower (2), so that the mixed fraction in the first rectification tower (2) flows into the secondary rectification device;
The inlet of the first circulating pump (3) is connected with the heavy component outlet of the first rectifying tower (2);
The outlet of the first circulating pump (3) is connected with the inlet of the first reboiler (4);
the outlet of the first reboiler (4) is connected with the light component inlet of the first rectifying tower (2);
an inlet of the first condenser (5) is connected with a light component outlet of the first rectifying tower (2), so that the light components CTF and TMP rectified and separated by the first rectifying tower (2) flow into the first condenser (5) to be condensed and liquefied;
the inlet of the first reflux vessel (6) is connected with the outlet of the first condenser (5), so that the liquefied CTF and TMP condensed by the first condenser (5) flows into the first reflux vessel (6) for storage;
an inlet of the first reflux pump (19) is connected with an outlet of the first reflux container (6), and an outlet of the first reflux pump (19) is connected with a reflux inlet of the first rectifying tower (2).
7. the apparatus for recovering ditrimethylolpropane according to claim 5,
The second-stage rectification device comprises a second rectification tower (7), a second circulating pump (8), a second reboiler (9), a second condenser (10), a second reflux container (11) and a second reflux pump (20), wherein,
The fraction inlet of the second rectifying tower (7) is connected with the primary rectifying device, so that the mixed fraction flows into the second rectifying tower (7);
the inlet of the second circulating pump (8) is connected with the heavy component outlet of the second rectifying tower (7);
The outlet of the second circulating pump (8) is connected with the inlet of the second reboiler (9);
the outlet of the second reboiler (9) is connected with the light component inlet of the second rectifying tower (7);
an inlet of the second condenser (10) is connected with a light component outlet of the second rectifying tower (7), so that the light components CTF and TMP rectified and separated by the second rectifying tower (7) flow into the second condenser (10) to be condensed and liquefied;
The inlet of the second reflux vessel (11) is connected with the outlet of the second condenser (10), so that the liquefied CTF and TMP condensed by the second condenser (10) flows into the second reflux vessel (11) for storage;
the inlet of the second reflux pump (20) is connected with the outlet of the second reflux container (11), and the outlet of the second reflux pump (20) is connected with the reflux inlet of the second rectifying tower (7).
8. the apparatus for recovering ditrimethylolpropane according to claim 5, further comprising:
the raw material pump (12) is connected between the acidification kettle (1) and the primary rectifying device, so that the mixed material in the acidification kettle (1) is pumped into the primary rectifying device;
and/or a heating device (13), wherein the heating device (13) is connected between the acidification kettle (1) and the primary rectification device and is used for heating the mixed material flowing into the primary rectification device from the acidification kettle (1);
and/or a third circulating pump (14), wherein the inlet of the third circulating pump (14) is connected with the circulating outlet of the acidification kettle (1), and the outlet of the third circulating pump (14) is connected with the circulating inlet of the acidification kettle (1) so as to enable the mixed material to circularly flow in the acidification kettle (1).
9. the apparatus for recovering ditrimethylolpropane according to claim 5,
the device is characterized by further comprising a vacuumizing device (17), wherein the vacuumizing device (17) is connected with the acidification kettle (1) and/or the primary rectifying device and/or the secondary rectifying device, so that the vacuumizing device (17) vacuumizes the acidification kettle (1) and/or the primary rectifying device and/or the secondary rectifying device.
10. the apparatus for recovering ditrimethylolpropane according to claim 9, wherein the vacuum extractor (17) is connected to the acidification still (1) and/or the primary rectification unit and/or the secondary rectification unit via a tail cooler (18).
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