CN117986217B - Phthalic anhydride raw material treatment method - Google Patents
Phthalic anhydride raw material treatment method Download PDFInfo
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- CN117986217B CN117986217B CN202410397495.XA CN202410397495A CN117986217B CN 117986217 B CN117986217 B CN 117986217B CN 202410397495 A CN202410397495 A CN 202410397495A CN 117986217 B CN117986217 B CN 117986217B
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- phthalic anhydride
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- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 title claims abstract description 130
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000002994 raw material Substances 0.000 title claims abstract description 52
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 168
- 238000001035 drying Methods 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000010828 elution Methods 0.000 claims description 23
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 238000005406 washing Methods 0.000 description 38
- 239000000203 mixture Substances 0.000 description 16
- 238000012216 screening Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012156 elution solvent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/87—Benzo [c] furans; Hydrogenated benzo [c] furans
- C07D307/89—Benzo [c] furans; Hydrogenated benzo [c] furans with two oxygen atoms directly attached in positions 1 and 3
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Furan Compounds (AREA)
Abstract
The invention discloses a phthalic anhydride raw material treatment method, which comprises the following steps: firstly, eluting and pre-treating unqualified phthalic anhydride raw materials with low untreated content by using a methanol eluting solvent, and then drying the raw materials at normal pressure to obtain high-content phthalic anhydride. The method can improve the content of phthalic anhydride products, has high yield, simple purification process of raw material treatment, low energy consumption, safety and environmental protection.
Description
Technical Field
The invention relates to a method for treating a high-content phthalic anhydride raw material, and belongs to the technical field of chemical industry.
Background
Phthalic anhydride is named phthalic anhydride, english abbreviation PA (Phthalic anhydride), which is an important basic organic chemical raw material, and is the variety with the largest production and consumption in tetraanhydride, more than 60% of which is used for manufacturing polyvinyl chloride plasticizer, 30% of which is used for polyester resin and alkyd resin, and the rest 10% of which is used for industries such as paint, dye, medicine and pesticide.
But phthalic anhydride has short shelf life and is easy to deteriorate into phthalic acid after the shelf life, so that a method for separating phthalic anhydride from phthalic acid is sought for reducing the cost; the recrystallization can separate phthalic acid and phthalic anhydride, but the steps are more complicated, and the consumed time and cost are higher.
Aiming at the raw materials with unqualified phthalic anhydride content, a phthalic anhydride raw material treatment method which has simple steps, lower cost and simple and convenient subsequent treatment is sought, and popularization and application are carried out.
Disclosure of Invention
At least aiming at the problems existing in the prior art, the invention provides a method for treating a high-content phthalic anhydride raw material, which can improve the content of phthalic anhydride products, has high yield, simple purification process of raw material treatment, low energy consumption, safety and environmental protection.
In order to achieve the above purpose, the present invention adopts the following technical scheme: a method for treating a high-content phthalic anhydride raw material comprises the following steps: firstly, eluting and pre-treating untreated raw materials with unqualified phthalic anhydride by using a methanol eluting solvent, and then drying the raw materials at normal pressure to obtain high-content phthalic anhydride.
Wherein, the conditions of elution pretreatment: and eluting for at least 3 times when the mass ratio of methanol to phthalic anhydride is 1:3-3:1 each time.
Preferably, the mass ratio of the methanol to the phthalic anhydride is 1:2-2:1.
Preferably, the mass ratio of the methanol to the phthalic anhydride is 1:1.
Preferably, the eluting is performed 3 to 5 times.
Preferably, the elution is 3 times.
Wherein, the normal pressure drying condition is as follows: the normal pressure drying temperature is 85-95 ℃, and the normal pressure drying time is 140-160 min.
Preferably, the above-mentioned normal pressure drying temperature is 90 ℃.
Preferably, the above-mentioned atmospheric drying time is 150 minutes.
Preferably, the purity of the unqualified phthalic anhydride raw material after treatment completely accords with AR grade, and the yield is more than 80 percent.
The invention has the beneficial effects that: the phthalic anhydride raw material treatment method of the invention is that the phthalic anhydride raw material with unqualified content is pretreated by methanol eluting solvent and then is dried at normal pressure, thus obtaining the phthalic anhydride with high content meeting AR grade requirement, and the content can reach 99.99 percent; meanwhile, the phthalic anhydride raw material treatment method also ensures that the phthalic anhydride has higher yield, and the yield is more than 80 percent; the phthalic anhydride raw material treatment method has the advantages of simple purification steps, easy operation, low cost, low energy consumption, safety and environmental protection; the phthalic anhydride raw material treatment method is suitable for industrial large-scale application.
Detailed Description
The following is a clear and complete description of the technical solutions in the practice of the present invention, and the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents, instruments and components used are conventional products commercially available without identifying the manufacturer.
Screening example 1 screening of drying conditions
500G of unqualified phthalic anhydride raw material with 98.6 percent of content is divided into 10 parts by weight without any treatment and respectively filled into glass crystallization dishes of the same type, and the glass crystallization dishes are evenly paved at the bottom of the glass crystallization dishes, wherein 5 parts of phthalic anhydride raw material is dried at different temperatures for different times under the condition of normal pressure (0.1013 MPa), 5 parts of phthalic anhydride raw material is dried at different temperatures for different times under the condition of reduced pressure (0.085 MPa), and the content of the phthalic anhydride raw material is detected, and the drying conditions and the product content change shown in table 1 are detected.
TABLE 1 screening of drying conditions
From the above Table 1, it was found that the phthalic anhydride content obtained by drying under normal pressure was greater than that obtained by drying under reduced pressure at the same temperature and time; at normal pressure and same time, the temperature is from 70 ℃ to 110 ℃, and the phthalic anhydride content is increased and then reduced along with the temperature rise; at normal pressure and the same temperature, the time is from 60min to 180min, and the phthalic anhydride content is increased and then reduced along with the time extension; therefore, the drying conditions are selected to be normal pressure and the temperature is 140-160 min at 85-95 ℃, so that the water easily adsorbed on the phthalic anhydride raw material due to the fact that the phthalic anhydride raw material is stored for too long can be efficiently removed, the phenomenon that the phthalic anhydride is hydrolyzed to generate impurities can be avoided, the drying conditions of the subsequent phthalic anhydride raw material subjected to material washing by using a solvent to remove the impurities are determined, the temperature is preferably 90 ℃ and the time is 150min, the phthalic anhydride has higher content, and meanwhile, the energy consumption is also saved.
Screening example 2 screening of elution solvent
Untreated 150g of unqualified phthalic anhydride raw material with the content of 98.6% is divided into 3 parts by weight, elution is carried out by using different eluting solvents respectively, elution is carried out for different times respectively, eluting solvents and phthalic anhydride are mixed according to the mass ratio of 1:1, eluting solvents are removed by using a centrifuge after each eluting, the drying is carried out for 150 minutes at the normal pressure and the temperature of 90 ℃, the content is detected, and the product yield is calculated by the weight after drying/the weight before eluting multiplied by 100%, and the eluting solvents, the eluting times, the product content and the product yield are shown in the table 2.
TABLE 2 screening of elution solvents
As shown in Table 2, the same eluting solvent showed a decrease in phthalic anhydride yield with increasing elution times, and the phthalic anhydride content was slightly decreased or maintained substantially unchanged after increasing gradually; it is also found that the consumption of phthalic anhydride is larger by adopting deionized water and absolute ethyl alcohol to wash the material, the impurity removing effect in the phthalic anhydride is poorer by adopting the deionized water, the impurity removing effect in the phthalic anhydride is better and the consumption of phthalic anhydride is small by adopting the methanol, but the content of the phthalic anhydride is lower when the methanol washing material is smaller than 3 times of phthalic anhydride; therefore, methanol is selected as an eluting solvent, and the eluting is carried out for 3-5 times, so that the phthalic anhydride purity reaches the AR (> 99.7%) level standard; preferably, the material is washed for 3 times, so that the phthalic anhydride has higher yield and simultaneously saves energy consumption.
Screening example 3 screening of the mass ratio of methanol to phthalic anhydride
Mixing and washing raw materials of the unqualified phthalic anhydride with the content of 98.6% of the raw materials of the methanol according to different mass ratios each time, removing the methanol by using a centrifugal machine after washing the raw materials, repeatedly eluting for 3 times, drying the raw materials at the temperature of 90 ℃ under normal pressure for 150 minutes, detecting the content of the raw materials of the phthalic anhydride, and calculating the yield of the raw materials, wherein the mass ratio of the methanol to the phthalic anhydride, the content of the product and the yield are shown in the table 3.
TABLE 3 screening of the mass ratio of methanol to phthalic anhydride
From the above table 3, it is found that when the material is washed, the mass ratio of methanol to phthalic anhydride is changed, the yield of phthalic anhydride is basically maintained unchanged, but the content of phthalic anhydride has a certain influence, when the ratio of methanol is too high, new impurities are easily introduced into phthalic anhydride, but when the ratio of methanol is too low, the material washing is insufficient, when the mass ratio of methanol to phthalic anhydride is more than 3:1 or less than 1:3, the content of phthalic anhydride is less than 99.7%, and the purity of phthalic anhydride does not reach the AR level standard; therefore, the mass ratio of methanol to phthalic anhydride is 1:3-3:1 during material washing, so that the phthalic anhydride content can be ensured to reach the AR level standard; preferably, the mass ratio of the methanol to the phthalic anhydride is 1:1.
Example 1
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 110g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 91.6g of phthalic anhydride with the yield of 83.3 percent and the content of 99.99 percent.
Example 2
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 150g of untreated unqualified phthalic anhydride with 98.6 percent of content is mixed with 150g of methanol for washing, the methanol is removed by a centrifugal machine after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 125.7g of phthalic anhydride with the yield of 83.8 percent and the content of 99.99 percent.
Example 3
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 110g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 4 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 90.6g of phthalic anhydride with the yield of 82.4 percent and the content of 99.98 percent.
Example 4
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 120g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 60g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 99.7g of phthalic anhydride with the yield of 83.1 percent and the content of 99.98 percent.
Example 4
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 120g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 40g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 99.9g of phthalic anhydride with the yield of 83.3 percent and the content of 99.96 percent.
Example 5
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 150g of untreated unqualified phthalic anhydride with 98.6 percent of content is mixed with 75g of methanol for washing, the methanol is removed by a centrifugal machine after the washing is finished, the repeated elution is carried out for 4 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 123.2g of phthalic anhydride with the yield of 82.1 percent and the content of 99.97 percent.
Example 6
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 150g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 75g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 5 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 121.2g of phthalic anhydride with the yield of 80.8 percent and the content of 99.96 percent.
Example 7
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 220g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 91.5g of phthalic anhydride with the yield of 83.2 percent and the content of 99.93 percent.
Example 8
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 80g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 240g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 150 minutes at the temperature of 90 ℃ under normal pressure to obtain 66.4g of phthalic anhydride with the yield of 83.0 percent and the content of 99.83 percent.
Example 9
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 110g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 160 minutes at the temperature of 90 ℃ under normal pressure to obtain 91.9g of phthalic anhydride with the yield of 83.6 percent and the content of 99.97 percent.
Example 10
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 110g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 140 minutes at the temperature of 95 ℃ under normal pressure to obtain 91.3g of phthalic anhydride with the yield of 83 percent and the content of 99.94 percent.
Example 11
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 110g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 3 times, and the mixture is dried for 160 minutes at the temperature of 85 ℃ under normal pressure to obtain 91.3g of phthalic anhydride with the yield of 83 percent and the content of 99.93 percent.
Example 12
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 110g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 4 times, and the mixture is dried for 140 minutes at the temperature of 85 ℃ under normal pressure to obtain 89.5g of phthalic anhydride with the yield of 81.4 percent and the content of 99.91 percent.
Example 13
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 110g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 4 times, and the mixture is dried for 160 minutes at the normal pressure and the temperature of 95 ℃ to obtain 88.9g of phthalic anhydride with the yield of 80.8 percent and the content of 99.92 percent.
Example 14
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 110g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 5 times, and the mixture is dried for 150 minutes at the temperature of 95 ℃ under normal pressure to obtain 88.7g of phthalic anhydride with the yield of 80.6 percent and the content of 99.94 percent.
Example 15
A method for treating high-content phthalic anhydride raw materials comprises the following specific processes: 110g of unqualified phthalic anhydride with the content of 98.6 percent which is not treated is mixed with 55g of methanol for washing, the methanol is removed by a centrifuge after the washing is finished, the repeated elution is carried out for 6 times, and the mixture is dried for 140 minutes at the temperature of 85 ℃ under normal pressure to obtain 88.3g of phthalic anhydride with the yield of 80.3 percent and the content of 99.89 percent.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (6)
1. A method for treating phthalic anhydride raw materials is characterized in that the method comprises the following steps: eluting raw phthalic anhydride with an untreated content of 98.6% by using a methanol eluting solvent, and then performing normal-pressure drying treatment to obtain phthalic anhydride with purity completely conforming to AR level, wherein the yield is more than 80%;
Conditions of the elution pretreatment: eluting for 3-5 times with the mass ratio of methanol to phthalic anhydride of 1:3-3:1 each time;
The normal pressure drying conditions are as follows: the normal pressure drying temperature is 85-95 ℃, and the normal pressure drying time is 140-160 min.
2. The method for treating phthalic anhydride raw material according to claim 1, wherein the mass ratio of methanol to phthalic anhydride is 1:2-2:1.
3. The method for treating phthalic anhydride as claimed in claim 2, wherein the mass ratio of methanol to phthalic anhydride is 1:1.
4. The method for treating phthalic anhydride as claimed in claim 1, wherein the elution is performed 3 times.
5. The method for treating phthalic anhydride as recited in claim 1, wherein the normal pressure drying temperature is 90 ℃.
6. The method for treating phthalic anhydride as recited in claim 5, wherein the normal pressure drying time is 150 minutes.
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