CN212713310U - Device for preparing alpha-chloro methyl palmitate from biodiesel - Google Patents
Device for preparing alpha-chloro methyl palmitate from biodiesel Download PDFInfo
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- CN212713310U CN212713310U CN202021744996.4U CN202021744996U CN212713310U CN 212713310 U CN212713310 U CN 212713310U CN 202021744996 U CN202021744996 U CN 202021744996U CN 212713310 U CN212713310 U CN 212713310U
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- tower
- chlorination
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- biodiesel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The utility model discloses a device with biodiesel preparation alpha-chloro palmitic acid methyl ester relates to biodiesel low reaches product development application technical field, has solved the problem that biodiesel's low reaches product added value is low among the prior art, and its technical essential is: the device comprises a rectifying tower, wherein the rectifying tower is connected with a filter press through a material pipe, the filter press is also connected with a mixer, the mixer is connected with a main chlorination tower and an auxiliary chlorination tower, an air outlet at the upper end of the main chlorination tower is connected with a feed inlet of the auxiliary chlorination tower, the feed inlet of the main chlorination tower is also connected with a chlorine gas source, and a discharge outlet of the auxiliary chlorination tower is also connected to the feed inlet of the main chlorination tower; the discharge port of the chlorination main tower is connected with an extraction tank, the extraction tank contains an extracting agent, and the discharge port of the extraction tank is connected with a drying tower; the utility model provides the added value of the accessory substance in the biodiesel preparation process is improved.
Description
Technical Field
The utility model relates to a biodiesel low reaches product development application technical field especially relates to a device with biodiesel preparation alpha-chloro palmitic acid methyl ester.
Background
With the vigorous development of the biodiesel industry, the application requirements of biodiesel are gradually improved, for example, the low-temperature performance is reflected in that the physical and chemical index is cloud point, and then methyl palmitate precipitated by condensation of a solution in the biodiesel needs to be fractionated and removed, so that the quality of the biodiesel is further improved.
Methyl chloropalmitate has good intermiscibility with PVC, excellent plasticizing effect, no toxicity, environmental protection, flame retardance, antistatic property and other excellent quality plasticizers, and is particularly suitable for the industries of cables and artificial leather.
In the prior art, the utilization rate of methyl palmitate is low, and the added value of the product is low, so a device for preparing alpha-chloro methyl palmitate by using biodiesel is provided.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to above-mentioned defect, provide a device with biodiesel preparation alpha-chloro methyl palmitate to solve among the prior art problem that biodiesel's low reaches product added value is low.
In order to achieve the above object, the utility model provides a following technical scheme:
a device for preparing alpha-chloro methyl palmitate by using biodiesel comprises a rectifying tower, wherein the rectifying tower is connected with a filter press through a material pipe, the filter press is also connected with a mixer, the mixer is connected with a chlorination main tower and a chlorination auxiliary tower, feed inlets and discharge outlets of the chlorination main tower and the chlorination auxiliary tower are respectively provided with a switch valve, an air outlet at the upper end of the chlorination main tower is connected with a feed inlet of the chlorination auxiliary tower, the feed inlet of the chlorination main tower is also connected with a chlorine gas source, and the discharge outlet of the chlorination auxiliary tower is also connected to the feed inlet of the chlorination main tower; the discharge port of the chlorination main tower is connected with an extraction tank, the extraction tank contains an extracting agent, and the discharge port of the extraction tank is connected with a drying tower.
As a further proposal of the utility model, the chlorination main tower and the chlorination auxiliary tower are both internally provided with high-pressure mercury lamps.
As a further scheme of the utility model, the upper end gas outlet of chlorination auxiliary tower still is connected with vapour and liquid separator, and vapour and liquid separator's discharge gate is connected with the backwash pump, and the backwash pump is connected to the feed inlet of chlorination auxiliary tower.
As a further proposal of the utility model, the gas outlet of the gas-liquid separator is also connected with an absorption tower which contains deionized water.
As a further proposal of the utility model, the absorption tower is also connected with a circulating pool.
To sum up, compared with the prior art, the utility model has the following beneficial effects:
1. the utility model discloses an adopt the product in the biodiesel rectification process to prepare high-purity alpha-chloro product for the plasticizer and the surfactant use can be regarded as to alpha-chloro product, have improved the added value of the accessory substance in the biodiesel preparation process.
2. The production process for producing the alpha-chloro product by adopting the utility model has simple flow, accurate chloro positioning, diversified product application, high purity of byproduct hydrochloric acid, environmental protection and no pollution in the production process.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing alpha-chloro methyl palmitate from biodiesel.
Reference numerals: the method comprises the following steps of 1-a rectifying tower, 2-a filter press, 3-a main chlorination tower, 4-a subsidiary chlorination tower, 5-an extraction tank, 6-a drying tower, 7-a gas-liquid separator, 8-an absorption tower, 9-a circulating pool and 10-a mixer.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative work belong to the protection scope of the present invention based on the embodiments of the present invention.
As shown in fig. 1, an apparatus for preparing alpha-chloro methyl palmitate from biodiesel comprises a rectifying tower 1, wherein the rectifying tower 1 is used for rectifying a biodiesel raw material, purifying the biodiesel and extracting a byproduct C16 methyl ester;
the rectifying tower 1 is connected with a filter press 2 through a material pipe, the filter press 2 is used for freezing and cleanly squeezing C16 methyl ester, so that the C16 methyl ester generates saturated methyl palmitate as a material of a next stage, the C16 methyl ester also generates a byproduct methyl palmitoleate in the filter press 2, the filter press 2 is also connected with a methyl palmitoleate collecting tank (not shown in the figure), and the methyl palmitoleate generated from the filter press 2 enters the methyl palmitoleate collecting tank;
the filter press 2 is further connected with a mixer 10, saturated methyl palmitate generated by the filter press 2 enters the mixer 10 and is mixed with a catalyst in the mixer 10, the mixer 10 is connected with a main chlorination tower 3 and an auxiliary chlorination tower 4, switch valves are arranged at feed inlets and discharge outlets of the main chlorination tower 3 and the auxiliary chlorination tower 4, the mixer 10 sends the mixed saturated methyl palmitate and the catalyst into the main chlorination tower 3 and the auxiliary chlorination tower 4 and performs a positioning chlorination reaction, high-pressure mercury lamps are arranged in the main chlorination tower 3 and the auxiliary chlorination tower 4 and are used for providing temperature and light for the positioning chlorination reaction; an air outlet at the upper end of the main chlorination tower 3 is connected with a feed inlet of the auxiliary chlorination tower 4, the feed inlet of the main chlorination tower 3 is also connected with a chlorine gas source, chlorine gas and saturated methyl palmitate are subjected to a positioning chlorination reaction in the main chlorination tower 3 under the action of a catalyst and the irradiation of a high-pressure mercury lamp, excessive chlorine gas and hydrogen chloride gas generated in the main chlorination tower 3 enter the auxiliary chlorination tower 4 through an air outlet at the upper end of the main chlorination tower 3 and are subjected to a positioning chlorination reaction with the saturated methyl palmitate in the auxiliary chlorination tower 4 under the action of the catalyst and the irradiation of the high-pressure mercury lamp, and the utilization rate of the chlorine gas can be improved by arranging the auxiliary chlorination tower 4, so that the material cost can be saved;
preferably, the discharge hole of the auxiliary chlorination tower 4 is also connected to the feed hole of the main chlorination tower 3, and when materials are added into the main chlorination tower 3, reaction products and reaction raw materials in the auxiliary chlorination tower 4 enter the main chlorination tower 3 to perform secondary reaction, so that the utilization rate of the raw materials is improved, and the raw materials are completely consumed;
the discharge port of the chlorination main tower 3 is connected with an extraction tank 5, the extraction tank 5 contains an extracting agent, the discharge port of the extraction tank 5 is connected with a drying tower 6, the extraction tank 5 is used for extracting alpha-chloro methyl palmitate in a reaction product in the chlorination main tower 3, after the chlorination main tower 3 is subjected to a positioned chlorination reaction, the chlorine content in the chlorination main tower 3 is detected, when the chlorine content in the chlorination main tower 3 reaches 11.66%, the positioned chlorination reaction in the chlorination main tower 3 reaches an end point, a feed inlet of the chlorination main tower 3 is closed, a discharge port of the chlorination main tower 3 is opened, materials in the chlorination main tower 3 enter the extraction tank 5, and after stirring, extraction, standing and layering, materials at the bottom layer of the extraction tank 5 are sent into the drying tower 6, and are subjected to vacuum dehydration by the drying tower 6 to prepare a product containing more than 95.0% of alpha-chloro methyl palmitate;
in some examples, the extractant is an 80% aqueous methanol solution;
in some examples, the catalyst is 2-thiopyridine-N-oxide.
As another embodiment of the invention, the gas outlet at the upper end of the auxiliary chlorination tower 4 is further connected with a gas-liquid separator 7, the discharge port of the gas-liquid separator 7 is connected with a reflux pump, the reflux pump is connected to the feed port of the auxiliary chlorination tower 4, the gas-phase material discharged from the auxiliary chlorination tower 4 enters the gas-liquid separator 7 and methyl ester is separated in the gas-liquid separator 7, and is added into the auxiliary chlorination tower 4 through the reflux pump and reacts with chlorine again in the auxiliary chlorination tower 4;
the gas outlet of the gas-liquid separator 7 is also connected with an absorption tower 8, the absorption tower 8 contains deionized water, the gas discharged from the gas outlet of the gas-liquid separator 7 is hydrogen chloride gas separated by the gas-liquid separator 7, and the hydrogen chloride gas discharged by the gas-liquid separator 7 enters the absorption tower 8 and is absorbed by the deionized water in the absorption tower 8 to generate hydrogen chloride solution;
the absorption tower 8 is further connected with a circulation tank 9, and the circulation tank 9 is used for circulating the deionized water in the absorption tower 8, so that the absorption tower 8 can continuously absorb hydrogen chloride gas.
A method for preparing alpha-chloro methyl palmitate by using biodiesel comprises the following steps:
s1, vacuum rectification, namely adding the biodiesel raw material into a rectification tower 1, controlling the temperature of a tower kettle in the rectification tower 1 at 195 ℃ and the pressure of the tower top at 100Pa, separating the biodiesel raw material into high-quality biodiesel with a low condensation point in the rectification tower 1 through vacuum rectification, and discharging C16 methyl ester from the tower top;
s2, cooling and crystallizing, namely, dishing and freezing the C16 methyl ester obtained in the S1 at the temperature of 10 ℃ in a mixer for 3 hours, filtering by a filter press 2 to obtain saturated methyl palmitate and methyl palmitoleate, and enabling the methyl palmitoleate generated in the filter press 2 to enter a methyl palmitoleate collecting tank;
s3, chlorination, namely feeding saturated methyl palmitate generated in the step S2 into a mixer 10, mixing and dissolving the saturated methyl palmitate and 2-thiopyridine-N-oxide in the mixer 10 and the 2-thiopyridine-N-oxide in proportion, then feeding the mixture into a main chlorination tower 3 and an auxiliary chlorination tower 4, controlling the temperature in the main chlorination tower 3 to be 70 ℃, feeding chlorine into the main chlorination tower 3, wherein the feeding time of the chlorine is 8 hours, stopping the reaction in the main chlorination tower 3 when the chlorine content in the main chlorination tower 3 reaches 11.66%, and controlling the temperature of the auxiliary chlorination tower 4 to be 65 ℃;
s4, a crude product purification process, wherein when the chlorine content in the chlorination main tower 3 reaches 11.66%, a discharge hole of the chlorination main tower 3 is opened, the materials in the chlorination main tower 3 are conveyed into an extraction tank 5, and then the materials in the chlorination auxiliary tower 4 are conveyed into the chlorination main tower 3 for continuous reaction; adding methanol aqueous solution with the weight of 20 percent of the alpha-chloro methyl palmitate into the extraction tank 5, stirring and extracting for 30min, standing and settling for 45min, separating out the lower oil layer, and introducing the oil layer into a drying tower 6 for gas evolution, dehydration and drying to obtain a reaction product.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The device for preparing the alpha-chloro methyl palmitate by using the biodiesel comprises a rectifying tower (1) and is characterized in that the rectifying tower (1) is connected with a filter press (2) through a material pipe, the filter press (2) is also connected with a mixer (10), the mixer (10) is connected with a main chlorination tower (3) and an auxiliary chlorination tower (4), the feed inlets and the discharge outlets of the main chlorination tower (3) and the auxiliary chlorination tower (4) are respectively provided with a switch valve, the gas outlet at the upper end of the main chlorination tower (3) is connected with the feed inlet of the auxiliary chlorination tower (4), the feed inlet of the main chlorination tower (3) is also connected with a chlorine gas source, and the discharge outlet of the auxiliary chlorination tower (4) is also connected to the feed inlet of the main chlorination tower (3); the discharge port of the chlorination main tower (3) is connected with an extraction tank (5), the extraction tank (5) contains an extracting agent, and the discharge port of the extraction tank (5) is connected with a drying tower (6).
2. The device for preparing alpha-chloro methyl palmitate with biodiesel according to claim 1, characterized in that the main chlorination tower (3) and the auxiliary chlorination tower (4) are both provided with high-pressure mercury lamps.
3. The device for preparing alpha-chloro methyl palmitate by using biodiesel according to claim 1 or 2, wherein the gas-liquid separator (7) is connected to the gas outlet at the upper end of the chlorination auxiliary tower (4), and the reflux pump is connected to the feed inlet of the chlorination auxiliary tower (4) and is connected to the discharge hole of the gas-liquid separator (7).
4. The device for preparing alpha-chloro methyl palmitate by using biodiesel according to claim 3, wherein the gas outlet of the gas-liquid separator (7) is further connected with an absorption tower (8), and the absorption tower (8) contains deionized water.
5. The plant for the production of methyl alpha-chloropalmitate from biodiesel according to claim 4, characterized in that said absorption column (8) is also connected to a circulation tank (9).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021744996.4U CN212713310U (en) | 2020-08-20 | 2020-08-20 | Device for preparing alpha-chloro methyl palmitate from biodiesel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021744996.4U CN212713310U (en) | 2020-08-20 | 2020-08-20 | Device for preparing alpha-chloro methyl palmitate from biodiesel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN212713310U true CN212713310U (en) | 2021-03-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202021744996.4U Expired - Fee Related CN212713310U (en) | 2020-08-20 | 2020-08-20 | Device for preparing alpha-chloro methyl palmitate from biodiesel |
Country Status (1)
| Country | Link |
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| CN (1) | CN212713310U (en) |
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2020
- 2020-08-20 CN CN202021744996.4U patent/CN212713310U/en not_active Expired - Fee Related
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210316 Termination date: 20210820 |