CN107814723A - The recovery method of triethylamine in a kind of permanent violet preparation process - Google Patents
The recovery method of triethylamine in a kind of permanent violet preparation process Download PDFInfo
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- CN107814723A CN107814723A CN201711120267.4A CN201711120267A CN107814723A CN 107814723 A CN107814723 A CN 107814723A CN 201711120267 A CN201711120267 A CN 201711120267A CN 107814723 A CN107814723 A CN 107814723A
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- triethylamine
- closed loop
- recovery method
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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- 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
- C09B19/00—Oxazine dyes
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Abstract
The invention provides a kind of recovery method of triethylamine in permanent violet preparation process, comprise the following steps：Closed loop product during preparing permanent violet as acid binding agent using triethylamine is provided；The pH value of the closed loop product obtained described in regulation, obtains alkaline system, the pH value of alkaline system is not less than 12；Alkaline system is distilled again, reclaim triethylamine, then through diafiltration, be dried to obtain permanent violet；The final temperature of the distillation is 105~120 DEG C, and the pressure of the distillation is normal pressure.Compared with the method for " end treatment " in the prior art, the invention belongs to watershed management, the pH value of closed loop product containing triethylamine hydrochloride is adjusted to more than 12, make triethylamine separate out, separated during triethylamine is united from system by distillation again, so as to greatly reduce the difficulty of diafiltration wastewater treatment and cost, and triethylamine energy Reusability is reclaimed, further reduce production cost.
Description
Technical field
The present invention relates to triethylamine recovery technical field, more particularly in a kind of permanent violet preparation process triethylamine return
Receiving method.
Background technology
Permanent violet belongs to dioxazine top grade organic pigment, has prominent tinctorial strength, brightness and excellent heat-resisting
Property, resistance to oozing property and good fastness to light, are coating, plastics, lucite, rubber, textile printing, aqueous ink, packages printing
Deng the well received pigment variety in field.
The current technique of permanent violet passes through condensation, closed loop mainly using 3- amino-N- ethyl carbazoles and tetrachloroquinone as raw material
It is prepared etc. series reaction step.Wherein, condensation step is mainly that 3- amino-N- ethyl carbazoles are contracted with tetrachloroquinone
Reaction is closed, needs to add acid binding agent triethylamine in the condensation reaction, the hydrogen chloride of neutralization reaction generation, promotes reaction to carry out.But
It is that the triethylamine added can cause to contain a large amount of triethylamine hydrochlorides in permanent violet production waste water, wastewater treatment difficulty is big, cost
Height, and the waste of triethylamine resource can be caused.Therefore, it is significant that triethylamine is reclaimed in permanent violet preparation process.
The content of the invention
In order to solve the problems, such as that permanent violet production wastewater treatment difficulty is big, cost is high, the invention provides a kind of permanent violet
The recovery method of triethylamine in preparation process, it can fully reclaim the triethylamine added as acid binding agent in reaction system.
The invention provides a kind of recovery method of triethylamine in permanent violet preparation process, comprise the following steps：
(1) the closed loop product during preparing permanent violet as acid binding agent using triethylamine is provided；
(2) pH value for the closed loop product that the step (1) obtains is adjusted, obtains alkaline system, the pH of the alkaline system
Value is not less than 12；
(3) alkaline system obtained to the step (2) distills, and reclaims triethylamine, obtains permanent violet；The distillation
Final temperature be 105~120 DEG C, the pressure of the distillation is normal pressure.
Preferably, in the step (2) the regulation temperature of pH value below 90 DEG C.
Preferably, using the pH value of strong base solution regulation closed loop product in the step (2).
Preferably, the mass concentration of the strong base solution is 5%~40%.
Preferably, the preparation method of the closed loop product comprises the steps of：
Using triethylamine as acid binding agent, 3- amino-N- ethyl carbazoles and tetrachloroquinone are subjected to condensation reaction, are condensed
Thing, the condensation reaction are carried out under the conditions of existing for organic solvent；
The obtained condensation product is mixed with benzene sulfonyl chloride, ring-closure reaction is carried out, obtains closed loop product.
Preferably, the temperature of the condensation reaction is 30~50 DEG C, and the time of the condensation reaction is 2~6h.
Preferably, the mass ratio of 3- amino-N- ethyl carbazoles, tetrachloroquinone and triethylamine is 1 in the condensation reaction:
0.6~0.8:0.4~0.6.
Preferably, the temperature of the ring-closure reaction is 160~180 DEG C, and the time of the ring-closure reaction is 2~6h.
Preferably, the mass ratio of benzene sulfonyl chloride and 3- amino-N- ethyl carbazoles is 0.4~0.6 in the ring-closure reaction:1.
The invention provides a kind of recovery method of triethylamine in permanent violet preparation process, comprise the following steps：There is provided with
Triethylamine prepares the closed loop product during permanent violet as acid binding agent；The pH value of the closed loop product obtained described in regulation, is obtained
The pH value of alkaline system, wherein alkaline system is not less than 12；Alkaline system is distilled again, reclaim triethylamine, then through diafiltration,
It is dried to obtain permanent violet.The present invention reclaims triethylamine during permanent violet is prepared, and is a kind of watershed management method, the present invention
The pH value of closed loop product containing triethylamine hydrochloride is adjusted to more than 12, makes triethylamine separate out, then incite somebody to action by distilling
Triethylamine is separated from system system, so as to greatly reduce the difficulty of diafiltration wastewater treatment and cost, and reclaims triethylamine
Energy Reusability, further reduces production cost.Compared with the method for " end treatment " in the prior art, side provided by the invention
The triethylamine recovery difficult that method can effectively avoid dissolving in waste liquid is relatively large and the problem of can not fully reclaiming, moreover it is possible to avoids
Residual of the triethylamine in permanent violet filter cake, and then thoroughly reclaim triethylamine.
Embodiment
The invention provides a kind of recovery method of triethylamine in permanent violet preparation process, comprise the following steps：
(1) the closed loop product during preparing permanent violet as acid binding agent using triethylamine is provided；
(2) pH value for the closed loop product that the step (1) obtains is adjusted, obtains alkaline system, the pH of the alkaline system
Value is not less than 12；
(3) alkaline system obtained to the step (2) distills, and reclaims triethylamine, obtains permanent violet；The distillation
Final temperature be 105~120 DEG C, the pressure of the distillation is normal pressure.
In the present invention, the preparation method of the closed loop product preferably comprises following steps：Using triethylamine as acid binding agent,
3- amino-N- ethyl carbazoles and tetrachloroquinone are subjected to condensation reaction, obtain condensation product, the condensation reaction is deposited in organic solvent
Carry out under the conditions；The obtained condensation product is mixed with benzene sulfonyl chloride, ring-closure reaction is carried out, obtains closed loop product.
The present invention preferably using triethylamine as acid binding agent, by 3- amino-N- ethyl carbazoles and tetrachloroquinone be condensed instead
Should, obtain condensation product.The present invention further preferably first 3- amino-N- ethyl carbazoles are mixed with organic solvent, obtain 3- amino-
N- ethyl carbazole solution, then tetrachloroquinone is added in the 3- amino-N- ethyl carbazole solution, obtains reaction system,
Carry out condensation reaction；Add triethylamine in the reaction system, in being carried out to acidic materials caused by the condensation reaction
With.In the present invention, the organic solvent is preferably o-dichlorohenzene.In the present invention, the organic solvent and 3- amino-N- second
The mass ratio of base carbazole is preferably 10~20:1, more preferably 12~18:1, more preferably 15:1.In the organic solvent
In, 3- amino-N- ethyl carbazoles can fully react with tetrachloroquinone, generate condensation product.
In the present invention, the mass ratio of the 3- amino-N- ethyl carbazoles, tetrachloroquinone and triethylamine is preferably 1:0.6
~0.8:0.4~0.6, more preferably 1:0.7:0.5.The present invention adds tetrachloroquinone in reaction system by several times, avoids
Reaction system caused by a large amount of tetrachloroquinones of disposable addition is sticky and can not stir, and influences the problem of reaction is carried out.
In the present invention, the addition temperature of the tetrachloroquinone is preferably 25~45 DEG C, more preferably 30~40 DEG C,
More preferably 35 DEG C.The present invention adds tetrachloroquinone at said temperatures, enables tetrachloroquinone and 3- amino-N- ethyl carbazoles
Fully react, control temperature in above range, avoid tetrachloroquinone activity it is higher caused by reaction system it is sticky, can not
The problem of stirring.
Triethylamine is preferably added in reaction system by the present invention in a manner of being added dropwise, and avoids adding a large amount of triethylamines simultaneously
Caused reaction is excessively violent, and reaction system viscosity is excessive, in the present invention, it is preferred to which the time control that triethylamine is added dropwise is 1
~2h.
In the present invention, the temperature of the condensation reaction is preferably 30~50 DEG C, more preferably 35~45 DEG C, is more entered
One step is preferably 40~45 DEG C；The time of the condensation reaction is preferably 2~6h, more preferably 3~5h, and more preferably 4
~5h.In the present invention, condensation generation acid occurs for the 3- amino-N- ethyl carbazoles and tetrachloroquinone, and triethylamine is anti-in condensation
Play a part of acid binding agent in answering, the acid of condensation generation is neutralized, reaction is smoothed out.
After obtaining condensation product, the present invention mixes the obtained condensation product with benzene sulfonyl chloride, carries out ring-closure reaction, obtains
Closed loop product.
In the present invention, the mass ratio of the benzene sulfonyl chloride and 3- amino-N- ethyl carbazoles is preferably 0.4~0.6:1, enter
One step is preferably 0.5:1.In the present invention, the mode of the mixing is preferably and the benzsulfamide is added in condensation product；
The addition temperature of the benzene sulfonyl chloride is preferably 120~140 DEG C, more preferably 125~135 DEG C, more preferably 130~
135℃。
In the present invention, the temperature of the ring-closure reaction is preferably 160~180 DEG C, more preferably 170~180 DEG C,
More preferably 175~180 DEG C.When the benzsulfamide is added into the mixing that raw material is realized by the way of condensation product, obtaining
After to the mixture of benzsulfamide and condensation product, reach described present invention preferably employs the mode that the mixture is heated up
Closed loop thermal.In the present invention, the time of the ring-closure reaction is preferably 2~6h, more preferably 3~5h, further
Preferably 4~5h.
After the ring-closure reaction, the pH value of the closed loop product obtained described in present invention regulation, alkaline system, the alkali are obtained
Property system pH value be not less than 12.
In the present invention, the regulation temperature of the pH value is more preferably 40~90 DEG C, more excellent preferably below 90 DEG C
Elect 70~90 DEG C as.
The present invention at said temperatures, adjusts the pH value of closed loop product, can effectively avoid boiling point due to triethylamine compared with
It is low so that dissociate the triethylamine rapid vaporization the problem of, while it also avoid that temperature is too low and sub-cooled caused by after
It is continuous to need extra heating and cause the energy and waste of time.
In the present invention, it is preferred to the pH value of closed loop product is adjusted using strong base solution.The strong base solution is preferably hydrogen-oxygen
Change sodium solution and/or potassium hydroxide solution；The mass concentration of the strong base solution is preferably 5%~40%, more preferably
10%~35%, it is still more preferably 20%~30%.The present invention using highly basic displacement weak base " principle, by closed loop product
PH value be adjusted to be not less than 12 so that the triethylamine in closed loop product cements out completely.
The present invention is not less than 12, preferably 12~14 using the pH value of strong base solution regulation closed loop product, further preferably
For 13~14.
The present invention is by the way that the pH value of closed loop product is adjusted to target zone so that the triethylamine in closed loop product is put completely
Swap out and.
After obtaining the alkaline system, the present invention distills to the obtained alkaline system, realizes returning for triethylamine
Receive, obtain permanent violet.
In the present invention, the final temperature of the distillation be 105~120 DEG C, preferably 110~120 DEG C, further preferably
For 115~120 DEG C, in the present invention, time of the distillation is controlled with the temperature of cut, i.e., to cut in still-process
Temperature is monitored in real time, when temperature reaches the final temperature of the distillation, stops distillation.In the present invention, the distillation
Pressure be normal pressure.
The present invention is under the vapo(u)rizing temperature so that and the triethylamine in alkaline system can be distilled sufficiently, then
The triethylamine that distillation obtains is reclaimed, realizes the re-using of triethylamine.
After the distillation, the present invention is preferably filtered the obtained permanent violet feed liquid, obtains permanent violet.The present invention
The filtering is not particularly limited, using filter operation well-known to those skilled in the art；In the implementation of the present invention
In example, the filtering is specially centrifuge rejection filter.
After the filtering, the filter cake obtained by preferred pair of the present invention is washed, and obtains pure permanent violet；The washing is excellent
Choosing is washed using o-dichlorohenzene and/or hot water to filter cake, and more preferably filter cake is carried out successively using o-dichlorohenzene
Primary washing and drying, obtain primary washing filter cake；Depth washing is carried out to the primary washing filter cake using hot water；The neighbour
The number of dichloro-benzenes washing is preferably 2~3 times, and the number of the hot wash is preferably clearly defined by the filtrate washed out.
The recovery method of triethylamine in a kind of permanent violet preparation process provided by the invention is carried out with reference to embodiment
Detailed description, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
300kg o-dichlorohenzenes and 30kg 3- amino-N- ethyl carbazoles are mixed, 18kg tetrachloros are added portionwise at 35 DEG C
Benzoquinones, 35 DEG C of temperature is controlled, throwing, which is finished, to be sealed, and continues stirring reaction 30 minutes；
In 1.5 hours, 12kg triethylamines are added dropwise, control 35 DEG C of temperature, continue stirring reaction at such a temperature 4 hours,
Obtain condensation product；
Condensation product is transferred to closed loop kettle, is warming up to 135 DEG C, 18kg benzene sulfonyl chlorides is added, is continuously heating to 175 DEG C, then
Back flow reaction 4 hours are incubated at 175 DEG C, obtain closed loop product；
After closed loop terminates, reaction system is cooled to 70 DEG C, liquid feeding alkali regulation pH to 12, is distilled to recover triethylamine, distillation
Final temperature be 105 DEG C.Collection obtains 9.8kg triethylamines, and the triethylamine that collection obtains is recycled.Be discharged to from
Scheming rejection filter, filter cake are first washed with o-dichlorohenzene at twice, and reusable heat water washing is clear to filtrate after drying, you can obtains filter cake
Permanent violet.After testing, triethylamine is free of in filtrate；Filter cake is through dry permanent violet 35.2kg, content 97.5%, at pigmentation
It is approximate with standard items (Δ E ＜ 0.5) to manage permanent violet finished product coloured light obtained by (kneading), relative color strength 101.2%.
Embodiment 2
300kg o-dichlorohenzenes and 30kg 3- amino-N- ethyl carbazoles are mixed, 24kg tetrachloros are added portionwise at 30 DEG C
Benzoquinones, 30 DEG C of temperature is controlled, throwing, which is finished, to be sealed, and continues stirring reaction 30 minutes；
In 1 hour, 12kg triethylamines are added dropwise, control 40 DEG C of temperature, continue stirring reaction at such a temperature 3 hours, obtain
Condensation product；
Condensation product is transferred to closed loop kettle, is warming up to 130 DEG C, benzene sulfonyl chloride 18kg is added, is continuously heating to 170 DEG C, then
Back flow reaction 3 hours are incubated at 170 DEG C, obtain closed loop product；
After closed loop terminates, reaction system is cooled to 90 DEG C, liquid feeding alkali regulation pH to 13, is distilled to recover triethylamine, distillation
Final temperature be 110 DEG C.Collection obtains 10.2kg triethylamines, and the triethylamine that collection obtains is recycled.
It is discharged to centrifuge rejection filter, filter cake is first washed with o-dichlorohenzene at twice, and reusable heat water washing is to filtrate after drying
Clearly, you can obtain permanent violet filter cake.After testing, triethylamine is free of in filtrate；Filter cake is through dry permanent violet 35.8kg, content
97.3%, approximate with standard items (Δ E ＜ 0.5), the relative color strength that handles permanent violet finished product coloured light obtained by (kneading) through pigmentation
100.5%.
Embodiment 3
600kg o-dichlorohenzenes and 30kg 3- amino-N- ethyl carbazoles are mixed, 18kg tetrachloros are added portionwise at 25 DEG C
Benzoquinones, 25 DEG C of temperature is controlled, throwing, which is finished, to be sealed, and continues stirring reaction 30 minutes；
In 2 hours, 18kg triethylamines are gradually added dropwise, control 30 DEG C of temperature, it is small to continue stirring reaction 2 at such a temperature
When, obtain condensation product；
Condensation product is transferred to closed loop kettle, is warming up to 120 DEG C, benzene sulfonyl chloride 18kg is added, is continuously heating to 160 DEG C, then
Back flow reaction 2 hours are incubated at 160 DEG C, obtain closed loop product；
After closed loop terminates, reaction system is cooled to 60 DEG C, liquid feeding alkali regulation pH to 13, is distilled to recover triethylamine, distillation
Final temperature be 115 DEG C.Collection obtains 15.6kg triethylamines, and the triethylamine that collection obtains is recycled.
It is discharged to centrifuge rejection filter, filter cake is first washed with o-dichlorohenzene at twice, and reusable heat water washing is to filtrate after drying
Clearly, you can obtain permanent violet filter cake.After testing, triethylamine is free of in filtrate；Filter cake is through dry permanent violet 34.6kg, content
97.8%, approximate with standard items (Δ E ＜ 0.5), the relative color strength that handles permanent violet finished product coloured light obtained by (kneading) through pigmentation
99.8%.
Embodiment 4
600kg o-dichlorohenzenes and 30kg 3- amino-N- ethyl carbazoles are mixed, 18kg tetrachloros are added portionwise at 45 DEG C
Benzoquinones, temperature 45 C is controlled, throwing, which is finished, to be sealed, and continues stirring reaction 30 minutes；
In 1.5 hours, 12kg triethylamines are added dropwise, control temperature 50 C, continue stirring reaction at such a temperature 5 hours,
Obtain condensation product；
Condensation product is transferred to closed loop kettle, is warming up to 140 DEG C, benzene sulfonyl chloride 12kg is added, is continuously heating to 180 DEG C, then
Back flow reaction 6 hours are incubated at 180 DEG C, obtain closed loop product；
After closed loop terminates, reaction system is cooled to 50 DEG C, liquid feeding alkali regulation pH to 14, is distilled to recover triethylamine, distillation
Final temperature be 120 DEG C.Collection obtains 10.3kg triethylamines, and the triethylamine that collection obtains is recycled.
It is discharged to centrifuge rejection filter, filter cake is first washed with o-dichlorohenzene at twice, and reusable heat water washing is to filtrate after drying
Clearly, you can obtain permanent violet filter cake.After testing, triethylamine is free of in filtrate；Filter cake is through dry permanent violet 36.1kg, content
98.2%, approximate with standard items (Δ E ＜ 0.5), the relative color strength that handles permanent violet finished product coloured light obtained by (kneading) through pigmentation
102.7%.
From the result of above example, the rate of recovery of triethylamine is high in permanent violet building-up process provided by the invention,
Triethylamine is free of in the permanent violet waste water obtained by recovery method of the present invention, and obtained by the method for the invention
Also triethylamine is free of in permanent violet filter cake, realizes the thorough recovery of triethylamine.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. the recovery method of triethylamine, comprises the following steps in a kind of permanent violet preparation process：
(1) the closed loop product during preparing permanent violet as acid binding agent using triethylamine is provided；
(2) pH value for the closed loop product that the step (1) obtains is adjusted, obtains alkaline system, the pH value of the alkaline system is not
Less than 12；
(3) alkaline system obtained to the step (2) distills, and reclaims triethylamine, obtains permanent violet；The end of the distillation
Only temperature is 105~120 DEG C, and the pressure of the distillation is normal pressure.
2. recovery method according to claim 1, it is characterised in that the regulation temperature of pH value is 90 in the step (2)
Below DEG C.
3. recovery method according to claim 1 or 2, it is characterised in that adjusted in the step (2) using strong base solution
The pH value of closed loop product.
4. recovery method according to claim 3, it is characterised in that the mass concentration of the strong base solution be 5%~
40%.
5. recovery method according to claim 1, it is characterised in that the preparation method of the closed loop product includes following step
Suddenly：
Using triethylamines as acid binding agent, 3- amino-N- ethyl carbazoles and tetrachloroquinone are subjected to condensation reaction, obtain condensation product,
The condensation reaction is carried out under the conditions of existing for organic solvent；
The obtained condensation product is mixed with benzene sulfonyl chloride, ring-closure reaction is carried out, obtains closed loop product.
6. recovery method according to claim 5, it is characterised in that the temperature of the condensation reaction is 30~50 DEG C, institute
The time for stating condensation reaction is 2~6h.
7. the recovery method according to claim 5 or 6, it is characterised in that 3- amino-N- ethyl clicks in the condensation reaction
The mass ratio of azoles, tetrachloroquinone and triethylamine is 1:0.6~0.8:0.4~0.6.
8. recovery method according to claim 5, it is characterised in that the temperature of the ring-closure reaction is 160~180 DEG C, institute
The time for stating ring-closure reaction is 2~6h.
9. the recovery method according to claim 5 or 8, it is characterised in that benzene sulfonyl chloride and 3- ammonia in the ring-closure reaction
The mass ratio of base-N- ethyl carbazoles is 0.4~0.6:1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711120267.4A CN107814723A (en) | 2017-11-14 | 2017-11-14 | The recovery method of triethylamine in a kind of permanent violet preparation process |
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| CN201711120267.4A CN107814723A (en) | 2017-11-14 | 2017-11-14 | The recovery method of triethylamine in a kind of permanent violet preparation process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111875977A (en) * | 2020-08-27 | 2020-11-03 | 银川百泓新材料科技有限公司 | Permanent violet refining system and method |
| CN112225750A (en) * | 2020-10-30 | 2021-01-15 | 安达市多森新材料科技有限公司 | Permanent violet preparation method with low wastewater discharge |
| CN116715586A (en) * | 2023-02-21 | 2023-09-08 | 福建紫金选矿药剂有限公司 | Recovery method of acid binding agent triethylamine in preparation process of 5-nonylsalicylaldehyde |
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| WO2002053654A2 (en) * | 2001-01-05 | 2002-07-11 | Sun Chemical Corporation | Preparation of heat stable pigment violet 23 |
| CN101817990A (en) * | 2010-05-04 | 2010-09-01 | 江西紫晶化学有限公司 | Method for synthesizing permanent violet |
| CN106430790A (en) * | 2016-11-22 | 2017-02-22 | 南京大学盐城环保技术与工程研究院 | Method for reducing COD (chemical oxygen demand) of permanent violet process wastewater and application of method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002053654A2 (en) * | 2001-01-05 | 2002-07-11 | Sun Chemical Corporation | Preparation of heat stable pigment violet 23 |
| CN101817990A (en) * | 2010-05-04 | 2010-09-01 | 江西紫晶化学有限公司 | Method for synthesizing permanent violet |
| CN106430790A (en) * | 2016-11-22 | 2017-02-22 | 南京大学盐城环保技术与工程研究院 | Method for reducing COD (chemical oxygen demand) of permanent violet process wastewater and application of method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111875977A (en) * | 2020-08-27 | 2020-11-03 | 银川百泓新材料科技有限公司 | Permanent violet refining system and method |
| CN111875977B (en) * | 2020-08-27 | 2023-10-31 | 银川百泓新材料科技有限公司 | Permanent violet refining system and refining method |
| CN112225750A (en) * | 2020-10-30 | 2021-01-15 | 安达市多森新材料科技有限公司 | Permanent violet preparation method with low wastewater discharge |
| CN116715586A (en) * | 2023-02-21 | 2023-09-08 | 福建紫金选矿药剂有限公司 | Recovery method of acid binding agent triethylamine in preparation process of 5-nonylsalicylaldehyde |
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Application publication date: 20180320 |