CN117776866A - Peach aldehyde byproduct recycling method - Google Patents
Peach aldehyde byproduct recycling method Download PDFInfo
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- CN117776866A CN117776866A CN202311582794.2A CN202311582794A CN117776866A CN 117776866 A CN117776866 A CN 117776866A CN 202311582794 A CN202311582794 A CN 202311582794A CN 117776866 A CN117776866 A CN 117776866A
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- peach aldehyde
- octanol
- recycling
- acid
- peach
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- 239000006227 byproduct Substances 0.000 title claims abstract description 70
- PHXATPHONSXBIL-UHFFFAOYSA-N xi-gamma-Undecalactone Chemical compound CCCCCCCC1CCC(=O)O1 PHXATPHONSXBIL-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004064 recycling Methods 0.000 title claims abstract description 20
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims abstract description 136
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000003377 acid catalyst Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 10
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940092714 benzenesulfonic acid Drugs 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000010410 layer Substances 0.000 claims abstract description 3
- 239000012044 organic layer Substances 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 30
- 238000001514 detection method Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 150000002148 esters Chemical class 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 4
- 238000004807 desolvation Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 244000144730 Amygdalus persica Species 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 244000242564 Osmanthus fragrans Species 0.000 description 2
- 235000019083 Osmanthus fragrans Nutrition 0.000 description 2
- 235000006040 Prunus persica var persica Nutrition 0.000 description 2
- 229920000180 alkyd Polymers 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- -1 cyclic lactone Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 2
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 description 2
- 235000003261 Artemisia vulgaris Nutrition 0.000 description 1
- 240000006891 Artemisia vulgaris Species 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 241000167854 Bourreria succulenta Species 0.000 description 1
- 244000241257 Cucumis melo Species 0.000 description 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 1
- 244000111489 Gardenia augusta Species 0.000 description 1
- 235000010254 Jasminum officinale Nutrition 0.000 description 1
- 240000005385 Jasminum sambac Species 0.000 description 1
- 240000007472 Leucaena leucocephala Species 0.000 description 1
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 1
- 244000018633 Prunus armeniaca Species 0.000 description 1
- 235000009827 Prunus armeniaca Nutrition 0.000 description 1
- 241000109463 Rosa x alba Species 0.000 description 1
- 235000005073 Rosa x alba Nutrition 0.000 description 1
- 241001104043 Syringa Species 0.000 description 1
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007036 catalytic synthesis reaction Methods 0.000 description 1
- 235000019693 cherries Nutrition 0.000 description 1
- 238000011208 chromatographic data Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- RHMZKSWPMYAOAZ-UHFFFAOYSA-N diethyl peroxide Chemical compound CCOOCC RHMZKSWPMYAOAZ-UHFFFAOYSA-N 0.000 description 1
- SRXOCFMDUSFFAK-UHFFFAOYSA-N dimethyl peroxide Chemical compound COOC SRXOCFMDUSFFAK-UHFFFAOYSA-N 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002978 peroxides Chemical group 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229940102001 zinc bromide Drugs 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of fine chemical industry, and discloses a peach aldehyde byproduct recycling method, which specifically comprises the following steps: adding byproducts generated in the synthesis of peach aldehyde into a reaction kettle, heating, then dripping an acid catalyst, cooling to normal temperature after thermal insulation decomposition, standing for layering, washing an upper organic layer, distilling to obtain octanol, recycling, and reusing, wherein the lower layer is the acid catalyst. According to the invention, sulfuric acid or benzenesulfonic acid water-soluble acid is used as a catalyst to treat the peach aldehyde by-product, and the peach aldehyde by-product is catalytically decomposed at a certain temperature, so that the effective components in the high-boiling-point by-product are decomposed, and excessive octanol is recovered through rectification for repeated use, thereby realizing comprehensive utilization of the peach aldehyde by-product, reducing the unit consumption of raw materials and increasing economic benefit.
Description
Technical Field
The invention belongs to the technical field of fine chemical industry, relates to recycling of industrial byproducts, and in particular relates to a peach aldehyde byproduct recycling method.
Background
Peach aldehyde, which is a colorless to pale yellow thick liquid with strong peach fragrance, is an important lactone spice, is commonly used in daily spices such as sweet osmanthus, jasmine, gardenia, mugwort, orange flower, white rose, syringa, acacia and the like, and is also a superior raw material for preparing food essence such as peach, melon, plum, apricot, cherry, osmanthus fragrans and the like. It is almost insoluble in water, soluble in ethanol and most common organic solvents, and can be widely used in daily use essence and edible essence.
At present, the peach aldehyde synthesis industry mainly uses acrylic acid (ester) and octanol to generate free radical reaction, and then the alkyd (ester) is generated, and then the alkyd (ester) is dehydrated or transesterified in a molecule to further generate cyclic lactone, and the free radical generation can be realized through thermal decomposition of peroxides (such as hydrogen peroxide, di-tert-butylalkyl methyl peroxide, ethyl peroxide and the like). For example, in the preparation method of peach aldehyde in patent CN116102527A, boric acid is used as a catalyst, an initiator triazine compound is added, a divalent nickel complex is added, and a light source with the wavelength range of 100-450 nm is adopted for catalytic synthesis of peach aldehyde. The method adopts an expensive divalent nickel complex as a catalyst and can realize catalysis only by the aid of a light source, so that the method is not suitable for industrial production. Patent CN102757411 reports that in the synthesis process using n-octanol and acrylic acid (ester) as raw materials, the initiator mainly comprises di-tert-butyl peroxide or benzoyl peroxide or tert-butyl hydroperoxide. The catalyst may be boric acid or zinc bromide. The method has the advantages that the product yield is about 80 percent, and the lower yield is caused by that the byproduct of the further reaction of the acrylic acid and the product is easily formed in the reaction, and the byproduct can be subjected to transesterification with the excessive octanol in the system to form a new byproduct. As shown in the following figure, in addition to the product peach aldehyde, the reaction of octanol with acrylic acid (ester) also forms peach aldehyde by-products A, B and C, which remain in the kettle liquid due to the relatively high molecular weight and the relatively high boiling point. Therefore, the kettle liquid rate of the reaction is greatly increased, and more economic loss is brought. Therefore, comprehensive utilization of these byproducts is also becoming an important research point for each company.
Many reports are about the improvement of the yield of peach aldehyde synthesis, but few reports about other side reactions are caused by the excessive use of octanol, and in practice, in the reaction, the byproduct rate (the byproduct quality: the finished product quality) is 20-30%, so that the production cost is high, the byproduct treatment amount is large, and the requirements on a three-waste treatment device are high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for recycling peach aldehyde byproducts, which takes sulfuric acid or benzenesulfonic acid water-soluble acid as a catalyst to treat the peach aldehyde byproducts and recover excessive octanol, thereby realizing the comprehensive utilization of the peach aldehyde byproducts, reducing the unit consumption of raw materials and increasing the economic benefit.
The invention is realized by the following technical scheme:
a peach aldehyde byproduct recycling method comprises the following steps:
adding byproducts generated in the synthesis of peach aldehyde into a reaction kettle, heating, then dripping an acid catalyst, cooling to normal temperature after thermal insulation decomposition, standing for layering, washing an upper organic layer, distilling to obtain octanol, recycling, and reusing, wherein the lower layer is the acid catalyst.
The invention further improves the scheme as follows:
a solvent is also added into the reaction kettle, wherein the solvent is C 1~ C 5 Mono-alcohols of (A)
Preferably, the solvent is one or more of methanol, ethanol or propanol.
Further, the mass of the solvent is 10% -20% of the mass of the byproduct.
Further, the acid catalyst is sulfuric acid or benzenesulfonic acid or a mixture of the sulfuric acid and benzenesulfonic acid.
Preferably, the acid catalyst is sulfuric acid with the mass concentration of 1% -20%.
Further, the mass of the catalyst is 10-50% of the mass of the byproduct.
Preferably, the mass of the catalyst is 30-50% of the mass of the byproduct.
Further, the temperature of thermal insulation decomposition is 100-300 ℃ and the time is 2-4 hours.
Preferably, the temperature of thermal insulation decomposition is 160-220 ℃.
The beneficial effects of the invention are as follows:
according to the invention, sulfuric acid or benzenesulfonic acid water-soluble acid is used as a catalyst to treat the peach aldehyde by-product, and the peach aldehyde by-product is catalytically decomposed at a certain temperature, so that the effective components in the high-boiling-point by-product are decomposed, octanol is recovered through crude distillation for repeated use, the comprehensive utilization of the peach aldehyde by-product is realized, the unit consumption of raw materials is reduced, and the economic benefit is increased.
The solvent used in the invention is C 1~ C 5 The alcohol is recycled in the course of crude distillation after decomposition reaction.
Drawings
FIG. 1 is data of chromatography prior to decomposition of peach aldehyde by-product;
figure 2 is chromatographic data after decomposition of peach aldehyde by-product.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
600g of peach aldehyde byproducts (the octanol content of which is lower than 2% in a meteorological chromatograph and the chromatograph is shown in figure 1) and 120g of 20% sulfuric acid are added into a 1L jacketed reaction kettle at normal temperature, the temperature is raised to 160 ℃ under stirring, the temperature is kept for 2-4 hours, the reaction liquid is sampled and subjected to meteorological chromatograph to show that the octanol content reaches 42.2% (chromatogram 2), the reaction liquid is distilled under reduced pressure to 180 ℃ under 2mmHg absolute pressure, the tower top fraction is 78.5g of products, the octanol content in the products is 84.1% in chromatographic detection, and the quality of the folded octanol accounts for 11.1% of the feeding quality of the peach aldehyde byproducts.
Example 2
600g of peach aldehyde byproducts (the octanol content of the meteorological chromatograph is less than 2 percent), 60g of sulfuric acid with 20 percent concentration, 120g of solvent ethanol and the like are added into a 1L jacketed reaction kettle at normal temperature, the temperature is raised to 200 ℃ under stirring, the temperature is kept for 2-4 hours, the octanol content reaches 45 percent by the meteorological chromatograph, the octanol is distilled to 180 ℃ under the absolute pressure of 2mmHg after the solvent is removed, the tower top fraction is 101.8g of products, the octanol content in the products detected by the chromatograph is 89.0 percent, and the quality of the folded octanol accounts for 15.3 percent of the feeding quality of the peach aldehyde byproducts.
Example 3
600g of peach aldehyde byproducts (the octanol content of the meteorological chromatograph is less than 2 percent), 120g of sulfuric acid with 20 percent concentration, 120g of solvent ethanol and the like are added into a 1L jacketed reaction kettle at normal temperature, the temperature is raised to 200 ℃ under stirring, the temperature is kept for 2-4 hours, the octanol content reaches 46 percent by the meteorological chromatograph, the octanol is distilled to 180 ℃ under the absolute pressure of 2mmHg after the solvent is removed, the tower top fraction is 112.1g of products, the octanol content in the products detected by the chromatograph is 91.2 percent, and the quality of the folded octanol accounts for 17.5 percent of the feeding quality of the peach aldehyde byproducts.
Example 4
600g (the octanol content of the meteorological chromatograph is less than 2 percent), 120g of sulfuric acid with 20 percent concentration is added into a 1L jacketed reaction kettle at normal temperature, the mixture is stirred and heated to 200 ℃ and then is kept for 2-4 hours, the meteorological chromatograph shows that the octanol content reaches 21 percent, the solvent is removed, the mixture is distilled under reduced pressure to 180 ℃ at the absolute pressure of 2mmHg, the tower top fraction is 43.6g of the product, the octanol content in the chromatographic detection product is 83.1 percent, and the quality of the folded octanol accounts for 6.2 percent of the feeding quality of the peach aldehyde byproduct.
Example 5
600g (the octanol content of the meteorological chromatograph is less than 2 percent), 300g of sulfuric acid with 20 percent concentration is added into a 1L jacketed reaction kettle at normal temperature, the mixture is stirred and heated to 200 ℃ and then is kept for 2-4 hours, the meteorological chromatograph shows that the octanol content reaches 52 percent, the mixture is decompressed and distilled to the kettle temperature of 180 ℃ under the absolute pressure of 2mmHg after the solvent is removed, the top fraction is 118.1g of the product, the octanol content in the chromatographic detection product is 86.2 percent, and the quality of the folded octanol accounts for 17.3 percent of the feeding quality of the peach aldehyde byproduct.
Example 6
600g (the octanol content of the meteorological chromatograph is less than 2 percent) of peach aldehyde byproducts, 300g of sulfuric acid with 10 percent concentration is added into a 1L jacketed reaction kettle at normal temperature, the mixture is stirred and heated to 200 ℃ and then is kept for 2-4 hours, the meteorological chromatograph shows that the octanol content reaches 52 percent, the solution is decompressed and distilled to the kettle temperature of 180 ℃ under the absolute pressure of 2mmHg after the solvent is removed, the tower top fraction is 116g of products, the octanol content in the products is 88 percent in chromatographic detection, and the quality of the folded octanol accounts for 17.2 percent of the feeding quality of the peach aldehyde byproducts.
Example 7
600g (the octanol content of the meteorological chromatograph is less than 2 percent) of peach aldehyde byproducts, 300g of sulfuric acid with 5 percent concentration are added into a 1L jacketed reaction kettle at normal temperature, the mixture is stirred and heated to 200 ℃ and then is kept for 2-4 hours, the meteorological chromatograph shows that the octanol content reaches 52 percent, the solution is decompressed and distilled to the kettle temperature of 180 ℃ under the absolute pressure of 2mmHg after the solvent is removed, the top fraction is 121g of products, the octanol content in the products is 84 percent in chromatographic detection, and the quality of the folded octanol accounts for 17.2 percent of the feeding quality of the peach aldehyde byproducts.
Example 8
600g (the octanol content of the meteorological chromatograph is less than 2 percent) of peach aldehyde byproducts, 300g of sulfuric acid with 1 percent concentration are added into a 1L jacketed reaction kettle at normal temperature, the mixture is stirred and heated to 200 ℃ and then is kept for 2-4 hours, the meteorological chromatograph shows that the octanol content reaches 48 percent, the mixture is decompressed and distilled to the kettle temperature of 180 ℃ under the absolute pressure of 2mmHg after the solvent is removed, the tower top fraction is 103g of products, the octanol content in the products detected by the chromatograph is 87.2 percent, and the quality of the folded octanol accounts for 15.3 percent of the feeding quality of the peach aldehyde byproducts.
Example 9
600g (the octanol content of the meteorological chromatograph is less than 2 percent) of peach aldehyde byproducts, 300g of sulfuric acid with 1 percent concentration is added into a 1L jacketed reaction kettle at normal temperature, the mixture is stirred and heated to 230 ℃ and then is kept for 2-4 hours, the meteorological chromatograph shows that the octanol content reaches 52 percent, the solution is decompressed and distilled to the kettle temperature of 180 ℃ under the absolute pressure of 2mmHg after the solvent is removed, the tower top fraction is 115.3g of products, the octanol content in the chromatographic detection products is 89.5 percent, and the quality of the folded octanol accounts for 17.3 percent of the feeding quality of the peach aldehyde byproducts.
Example 10 (first time acid)
600g of peach aldehyde byproduct (the octanol content of the meteorological chromatograph is less than 2%) is added into a 1L jacketed reaction kettle at normal temperature, 260g of the stratified aqueous phase of the embodiment 9 and the stratified aqueous phase of sulfuric acid of the overhead fraction are added into the reaction kettle, the temperature is raised to 230 ℃ under stirring, the temperature is kept for 2-4 hours, the octanol content is up to 52% under the meteorological chromatograph, the octanol is distilled to 180 ℃ under the reduced pressure under the absolute pressure of 2mmHg after the desolvation, the overhead fraction is 127.3g of the product, the octanol content in the chromatographic detection product is 89.5%, and the quality of the folded octanol accounts for 19.2% of the feeding quality of the peach aldehyde byproduct.
Example 11 (second time acid application)
600g of peach aldehyde byproduct (the octanol content of the meteorological chromatograph is less than 2%) is added into a 1L jacketed reaction kettle at normal temperature, 230g of the stratified aqueous phase of the embodiment 10 and the stratified aqueous phase of sulfuric acid of the overhead fraction are added into the reaction kettle, the temperature is raised to 230 ℃ under stirring, the temperature is kept for 2-4 hours, the octanol content is 50% by the meteorological chromatograph, the octanol is distilled to 180 ℃ under reduced pressure under the absolute pressure of 2mmHg after the desolvation, the overhead fraction is 125.6g of the product, the octanol content in the chromatographic detection product is 89.5%, and the quality of the folded octanol accounts for 18.7% of the feeding quality of the peach aldehyde byproduct.
Example 12 (fifth time acid)
600g of peach aldehyde byproducts (the octanol content of the meteorological chromatograph is lower than 2%) are added into a 1L jacketed reaction kettle at normal temperature, 150g of layering water phase and 150g of tower top water phase which are used for the fourth time are added into the reaction kettle, 150g of sulfuric acid with 1% concentration is added, the temperature is raised to 230 ℃ under stirring, the temperature is kept for 2-4 hours, the meteorological chromatograph shows that the octanol content reaches 50%, the absolute pressure of 2mmHg is reduced pressure and distilled to 180 ℃ after the desolvation, the tower top fraction is 123.9g of products, the octanol content in the products is detected by the chromatograph, and the quality of the folded octanol accounts for 18.3% of the feeding quality of the peach aldehyde byproducts.
Example 13 (tenth time acid application)
600g of peach aldehyde byproducts (the octanol content of the meteorological chromatograph is lower than 2%) is added into a 1L jacketed reaction kettle at normal temperature, 170g of the layered water phase and the top water phase which are used for the ninth time are added into the reaction kettle, 150g of water is added, the temperature is raised to 230 ℃ under stirring, the temperature is kept for 2-4 hours, the octanol content reaches 52% under the meteorological chromatograph, the octanol is distilled to 180 ℃ under the absolute pressure of 2mmHg after the desolvation, the top fraction is 129.6g of products, the octanol content in the products detected by the chromatograph is 87.2%, and the quality of the folded octanol accounts for 18.8% of the feeding quality of the peach aldehyde byproducts.
The foregoing embodiments are merely illustrative of the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement the same, not to limit the scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.
Claims (10)
1. The peach aldehyde byproduct recycling method is characterized by comprising the following steps of: adding byproducts generated in the synthesis of peach aldehyde into a reaction kettle, heating, then dripping an acid catalyst, cooling to normal temperature after thermal insulation decomposition, standing for layering, washing an upper organic layer, distilling to obtain octanol, recycling, and reusing, wherein the lower layer is the acid catalyst.
2. The method for recycling peach aldehyde byproducts according to claim 1, which is characterized in that: a solvent is also added into the reaction kettle, wherein the solvent is C 1~ C 5 Is a mono-alcohol of (a).
3. The method for recycling peach aldehyde byproducts according to claim 2, which is characterized in that: the solvent is one or more of methanol, ethanol or propanol.
4. A peach aldehyde byproduct recycling method according to claim 2 or 3, characterized in that: the mass of the solvent is 10% -20% of the mass of the byproduct.
5. The method for recycling peach aldehyde byproducts according to claim 1, which is characterized in that: the acid catalyst is sulfuric acid or benzenesulfonic acid or a mixture of the sulfuric acid and benzenesulfonic acid.
6. The method for recycling peach aldehyde byproducts according to claim 5, which is characterized in that: the acid catalyst is sulfuric acid with the mass concentration of 1% -20%.
7. The method for recycling peach aldehyde byproducts according to claim 1, which is characterized in that: the mass of the catalyst is 10-50% of the mass of the byproduct.
8. The method for recycling peach aldehyde byproducts according to claim 7, wherein: the mass of the catalyst is 30-50% of the mass of the byproduct.
9. The method for recycling peach aldehyde byproducts according to claim 1, which is characterized in that: the temperature of thermal insulation decomposition is 100-300 ℃ and the time is 2-4 hours.
10. The method for recycling peach aldehyde byproducts according to claim 9, wherein the method comprises the following steps: the temperature of thermal insulation decomposition is 160-220 ℃.
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| CN202311582794.2A CN117776866A (en) | 2023-11-24 | 2023-11-24 | Peach aldehyde byproduct recycling method |
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| CN202311582794.2A CN117776866A (en) | 2023-11-24 | 2023-11-24 | Peach aldehyde byproduct recycling method |
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| Country | Link |
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