CN1086526A - Simple and feasible phthalocyanine copper manufacturing method - Google Patents
Simple and feasible phthalocyanine copper manufacturing method Download PDFInfo
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- CN1086526A CN1086526A CN 92112674 CN92112674A CN1086526A CN 1086526 A CN1086526 A CN 1086526A CN 92112674 CN92112674 CN 92112674 CN 92112674 A CN92112674 A CN 92112674A CN 1086526 A CN1086526 A CN 1086526A
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- CN
- China
- Prior art keywords
- prior
- art
- thermophore
- clumps
- trees
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000004519 manufacturing process Methods 0.000 title claims description 10
- VVOPUZNLRVJDJQ-UHFFFAOYSA-N phthalocyanine copper Chemical compound [Cu].C12=CC=CC=C2C(N=C2NC(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2N1 VVOPUZNLRVJDJQ-UHFFFAOYSA-N 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 7
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 20
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 9
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 9
- 241001330002 Bambuseae Species 0.000 claims description 9
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 9
- 239000011425 bamboo Substances 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 5
- 229940010552 ammonium molybdate Drugs 0.000 claims description 5
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 5
- 239000011609 ammonium molybdate Substances 0.000 claims description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 5
- 229940045803 cuprous chloride Drugs 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229940045136 urea Drugs 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 abstract 2
- 230000007547 defect Effects 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical class N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 239000000975 dye Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- QXJJQWWVWRCVQT-UHFFFAOYSA-K calcium;sodium;phosphate Chemical compound [Na+].[Ca+2].[O-]P([O-])([O-])=O QXJJQWWVWRCVQT-UHFFFAOYSA-K 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000000414 obstructive effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B47/00—Porphines; Azaporphines
- C09B47/04—Phthalocyanines abbreviation: Pc
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The copper phthalocyanine product is one of important varieties in the dye industry and is also a basic intermediate of phthalocyanine series products. The invention aims to overcome the defects of the prior art that effective collision and contact opportunities among reactant molecules are few, namely the reaction period is long, and the yield and the quality are low. The invention adopts the steps of heating and melting phthalic anhydride, urea and a catalyst to form a mixed molecular state, uniformly stirring, mixing with a heat carrier, stirring and heating to a reaction temperature to obtain the copper phthalocyanine with qualified purity. Compared with the prior art, the invention shortens the reaction period by about ten times, reduces the raw material cost by about 10 percent, reduces the heat energy and the electric energy by about 50 percent, has simpler equipment and operation than the prior art, and has no toxicity.
Description
The invention belongs to the chemical dyestuff field.
Phthalein mountain valley with clumps of trees and bamboo copper is a kind of dyestuff, also is the intermediate of phthalein mountain valley with clumps of trees and bamboo series dyes, pigment.Because its premium properties and use are widely had a preference for by the producers and consumers, but not good enough owing to production method, have limited its output, quality and consumption always.
At present, according to the available data report, the production method of phthalein mountain valley with clumps of trees and bamboo copper is all based on solvent method and solid phase burning method both at home and abroad.The shortcoming of solvent method is: 1. because the obstructive action of solvent make reactant molecule be difficult for contact and formation molecule, so reaction time is long; 2. some solvent also produces deleterious by product, as polychlorobiphenyl, influences products export.The shortcoming of solid phase roasting method is because solid materials mixes, and is fusion when roasting, can not stir, so mix inequality between every kind of molecule, the molecule of some pre-reaction does not contact, so output and content are all low.
Purpose of the present invention and task are that the common weakness that solves above-mentioned two kinds of production methods proposes.
Implementation method of the present invention is as follows:
Earlier with raw material phthalic anhydride, urea, cuprous chloride, ammonium molybdate by 12: 18: 2: 0.1 proportioning fusion or dissolve, and fully stirring make its raw material uniform mixing; For the molecule that makes the pre-reaction raw material reaches temperature of reaction rapidly, adopt thermophore.Thermophore can be that solid also can be a liquid; Thermophore is heated to temperature required about 150 ℃, said mixture is under agitation slowly poured thermal barrier in the mixed solution then again, through heat up, insulation, again through dilute sulphuric acid and water washing to neutral, filter, oven dry, pulverize, phthalein mountain valley with clumps of trees and bamboo copper finished product.
Technical process such as accompanying drawing 1.
Mixed uniformly raw material and catalyzer mix back formation several raw material spheroids with the glass sphere center with hot glass sphere (thermophore), distance is very near between raw material on these spherome surfaces and the catalyst molecule, under the situation of inside and outside heating, pass through rapidly the differing temps stage, and make raw molecule be varied to phthalein mountain valley with clumps of trees and bamboo copper through intermediate product.Can avoid the deficiency of solvent method and solid phase roasting method.Its reaction formula is as follows:
Thermophore can be a solid, also can be liquid, but must be fusing point or boiling point higher not with the material of raw material react with, and want separate easily.
Use this method, can avoid the intermolecular contact of solvent taraxy thing of solvent method and production cycle that collision causes long, it is uneven also can to avoid the part raw molecule of roasting method to mix, not have to collide and yield that contact conditions causes low, content is low.
Advantage of the present invention is as follows: (with solvent method and solid phase method ratio)
1, the production cycle is 1～2 hour, and the output and the scale of product is changeable (be 20 hours the reaction time of solvent method);
2, equipment is simple and easy to make, less investment, and floor space is few;
3, the comparable solvent method of products material cost is low by about 10%, without solvent without alkali;
4, heat energy and electric energy reduce about 50% than solvent method, heating time of concentration weak point, and product does not contain Toxic matter.Under the good situation of whole technology controlling and process, also can be without pickling.
Provide embodiments of the invention below:
Phthalic anhydride 12g, urea matter 18g, cuprous chloride 2.1g, ammonium molybdate 0.1g, 100 milliliters of glass spheres (thermophore) (2～3 millimeters of diameters).
Operation steps is:
(1). glass sphere is heated to 150 ℃ waits to do.
(2). get phthalic anhydride 12g, urea 18g splashes into the wetting fine melt that is heated to of little water, adds cuprous chloride 2.1g and ammonium molybdate 0.1g again, and brute force stirs.
(3). under agitation, be heated to 200 ± 5 ℃, be incubated about 10 minutes, lower the temperature then below 100 ℃ with moderate heat with the hot glass sphere of previously prepd pouring in the mixed liquor slowly.
(4). will react material well and use dilute sulphuric acid (about 50%) to soak about 30 minutes, and stir filtered while hot, and wash neutrality, dry, get phthalein mountain valley with clumps of trees and bamboo copper 9.7g, and analyze content 93%, coloured light and reference colour are approximate.
Claims (3)
1, a kind of manufacture method of phthalein mountain valley with clumps of trees and bamboo copper is characterized in that: with raw material phthalic anhydride, urea, cuprous chloride, ammonium molybdate in 12: 18: 2: 0.1 ratio dissolves or melts, and fully stirs, and makes its uniform mixing.
2, the manufacture method of phthalein mountain valley with clumps of trees and bamboo copper as claimed in claim 1 is characterized in that: for the raw molecule that makes pre-reaction reaches temperature of reaction rapidly, adopt thermophore.And thermophore can be that solid also can be a liquid.
3, as the manufacture method of claim 1 and 2 described phthalein mountain valley with clumps of trees and bamboo copper, it is characterized in that: thermophore is slowly poured in the mixed solution of under agitation phthalic anhydride, urea, cuprous chloride, ammonium molybdate, uniform mixing is heated to and reacts completely.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92112674 CN1086526A (en) | 1992-11-02 | 1992-11-02 | Simple and feasible phthalocyanine copper manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92112674 CN1086526A (en) | 1992-11-02 | 1992-11-02 | Simple and feasible phthalocyanine copper manufacturing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1086526A true CN1086526A (en) | 1994-05-11 |
Family
ID=4946052
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92112674 Pending CN1086526A (en) | 1992-11-02 | 1992-11-02 | Simple and feasible phthalocyanine copper manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1086526A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376109B (en) * | 2008-09-22 | 2010-04-21 | 宣城亚邦化工有限公司 | Sodium-molybdenum series composite catalyst for synthesizing copper phthalocyanine |
| CN106964407A (en) * | 2017-03-28 | 2017-07-21 | 齐鲁工业大学 | A kind of CuPc/γ bismuth molybdate composite nano fiber catalysis materials and preparation method and application |
-
1992
- 1992-11-02 CN CN 92112674 patent/CN1086526A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101376109B (en) * | 2008-09-22 | 2010-04-21 | 宣城亚邦化工有限公司 | Sodium-molybdenum series composite catalyst for synthesizing copper phthalocyanine |
| CN106964407A (en) * | 2017-03-28 | 2017-07-21 | 齐鲁工业大学 | A kind of CuPc/γ bismuth molybdate composite nano fiber catalysis materials and preparation method and application |
| CN106964407B (en) * | 2017-03-28 | 2019-05-28 | 齐鲁工业大学 | A kind of CuPc/γ-bismuth molybdate composite nano fiber catalysis material and the preparation method and application thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |