CN114316629A - Green and environment-friendly disperse dye intermediate treatment method - Google Patents
Green and environment-friendly disperse dye intermediate treatment method Download PDFInfo
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- CN114316629A CN114316629A CN202111587880.3A CN202111587880A CN114316629A CN 114316629 A CN114316629 A CN 114316629A CN 202111587880 A CN202111587880 A CN 202111587880A CN 114316629 A CN114316629 A CN 114316629A
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Abstract
The invention relates to the technical field of disperse dye intermediate treatment, in particular to a green environment-friendly disperse dye intermediate treatment method, which comprises the following steps: pretreating an environment-friendly disperse dye intermediate; step two: adding water into the disperse dye intermediate; step three: acid treatment of the disperse dye intermediate; step four: heating reaction of the disperse dye intermediate; step five: distilling the disperse dye intermediate; step six: cooling; step seven: the invention has the beneficial effects that by adding the auxiliary agent: impurity in can giving the disperse dyes through the filtration to disperse dyes and getting rid of and then get rid of some harmful substance in the disperse dyes, then make the content that can effectual reduction chlorobenzene and chlorotoluene in the disperse dyes and then make the content of chlorobenzene and chlorotoluene reach the operation requirement in market in the disperse dyes through reacting it with acid at high temperature, this processing method simply effectively makes the more environmental protection of disperse dyes after handling.
Description
Technical Field
The invention relates to the technical field of disperse dye intermediate treatment, in particular to a method for treating a green environment-friendly disperse dye intermediate.
Background
The disperse dye intermediate is also called intermediate, which is a general term for various aromatic hydrocarbon derivatives used for producing dyes and organic pigments, and is prepared by taking aromatic hydrocarbons such as benzene, toluene, naphthalene, anthracene and the like from coal chemical industry and petrochemical industry as basic raw materials through a series of organic synthesis unit processes.
Disclosure of Invention
The invention aims to provide a method for processing an intermediate of a green environment-friendly disperse dye, which is used for solving the problems in the process.
In order to achieve the purpose, the invention provides the following technical scheme: a method for processing an intermediate of a green environment-friendly disperse dye, which comprises the following steps,
a green environment-friendly disperse dye intermediate treatment method comprises the following steps:
the method comprises the following steps: pretreatment of the environment-friendly disperse dye intermediate: filtering the environment-friendly disperse dye intermediate to remove impurities in the disperse dye intermediate;
step two: adding water to disperse dye intermediate: adding a certain amount of water into the intermediate of the disperse dye, and fully stirring;
step three: acid addition treatment of the disperse dye intermediate: adding a certain amount of acid into the mixed solution obtained in the step two, and fully stirring to uniformly mix the mixed solution;
step four: heating reaction of the disperse dye intermediate: fully reacting the mixed solution obtained in the third step at different temperatures;
step five: distillation of the disperse dye intermediate: distilling the mixed solution after the reaction in the fourth step;
step six: cooling treatment: cooling the disperse dye intermediate obtained in the fifth step to restore the temperature of the disperse dye intermediate to a normal temperature state;
step seven: addition of auxiliary agents: and adding a dispersing agent and a bactericide into the disperse dye intermediate recovered to the normal temperature, fully stirring and filtering.
Preferably, the filtering treatment in the first step is to perform fine filtration on the disperse dye intermediate by using a multi-layer filter to remove impurities in the disperse dye intermediate.
Preferably, the mass ratio of the water added in the second step to the disperse dye intermediate is 1: 10-45.
Preferably, the mass ratio of the acid added in the third step to the disperse dye intermediate is 1: 2-8.
Preferably, the temperature conditions in the fourth step are different and range from 70 ℃ to 135 ℃, and the reaction time is 2.5 hours to 7 hours.
Preferably, the dispersant in the seventh step is one or both of polypropylene dilute hydrochloric acid and polymethyl methacrylate dilute hydrochloric acid, and the bactericide is sodium benzoate.
Compared with the prior art, the invention has the beneficial effects that: impurity in can giving the disperse dyes through the filtration to disperse dyes and getting rid of and then get rid of some harmful substance in the disperse dyes, then make the content that can effectual reduction chlorobenzene and chlorotoluene in the disperse dyes and then make the content of chlorobenzene and chlorotoluene reach the operation requirement in market in the disperse dyes through reacting it with acid at high temperature, this processing method simply effectively makes the more environmental protection of disperse dyes after handling.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A green environment-friendly disperse dye intermediate treatment method comprises the following steps:
the method comprises the following steps: pretreatment of the environment-friendly disperse dye intermediate: filtering the environment-friendly disperse dye intermediate to remove impurities in the disperse dye intermediate;
step two: adding water to disperse dye intermediate: adding a certain amount of water into the intermediate of the disperse dye, and fully stirring;
step three: acid addition treatment of the disperse dye intermediate: adding a certain amount of acid into the mixed solution obtained in the step two, and fully stirring to uniformly mix the mixed solution;
step four: heating reaction of the disperse dye intermediate: fully reacting the mixed solution obtained in the third step at different temperatures;
step five: distillation of the disperse dye intermediate: distilling the mixed solution after the reaction in the fourth step;
step six: cooling treatment: cooling the disperse dye intermediate obtained in the fifth step to restore the temperature of the disperse dye intermediate to a normal temperature state;
step seven: addition of auxiliary agents: and adding a dispersing agent and a bactericide into the disperse dye intermediate recovered to the normal temperature, fully stirring and filtering.
Wherein:
and the filtering treatment in the first step is to adopt a multilayer filter to carry out precise filtration on the disperse dye intermediate to remove impurities in the disperse dye intermediate.
And the mass ratio of the water added in the second step to the disperse dye intermediate is 1: 15.
The mass ratio of the acid added in the third step to the disperse dye intermediate is 1: 2.
The temperature range in the fourth step is 70 ℃, and the reaction time is 2.5 hours.
And the dispersant in the seventh step is a mixture of polypropylene dilute hydrochloric acid and polymethyl methacrylate dilute hydrochloric acid, and the bactericide is sodium benzoate.
Example two
A green environment-friendly disperse dye intermediate treatment method comprises the following steps:
the method comprises the following steps: pretreatment of the environment-friendly disperse dye intermediate: filtering the environment-friendly disperse dye intermediate to remove impurities in the disperse dye intermediate;
step two: adding water to disperse dye intermediate: adding a certain amount of water into the intermediate of the disperse dye, and fully stirring;
step three: acid addition treatment of the disperse dye intermediate: adding a certain amount of acid into the mixed solution obtained in the step two, and fully stirring to uniformly mix the mixed solution;
step four: heating reaction of the disperse dye intermediate: fully reacting the mixed solution obtained in the third step at different temperatures;
step five: distillation of the disperse dye intermediate: distilling the mixed solution after the reaction in the fourth step;
step six: cooling treatment: cooling the disperse dye intermediate obtained in the fifth step to restore the temperature of the disperse dye intermediate to a normal temperature state;
step seven: addition of auxiliary agents: and adding a dispersing agent and a bactericide into the disperse dye intermediate recovered to the normal temperature, fully stirring and filtering.
Wherein:
and the filtering treatment in the first step is to adopt a multilayer filter to carry out precise filtration on the disperse dye intermediate to remove impurities in the disperse dye intermediate.
And the mass ratio of the water added in the second step to the disperse dye intermediate is 1: 20.
The mass ratio of the acid added in the third step to the disperse dye intermediate is 1: 3.
The temperature in the fourth step is different and ranges from 80 ℃, and the reaction time is 3 hours.
And the dispersant in the seventh step is a mixture of polypropylene dilute hydrochloric acid and polymethyl methacrylate dilute hydrochloric acid, and the bactericide is sodium benzoate.
EXAMPLE III
A green environment-friendly disperse dye intermediate treatment method comprises the following steps:
the method comprises the following steps: pretreatment of the environment-friendly disperse dye intermediate: filtering the environment-friendly disperse dye intermediate to remove impurities in the disperse dye intermediate;
step two: adding water to disperse dye intermediate: adding a certain amount of water into the intermediate of the disperse dye, and fully stirring;
step three: acid addition treatment of the disperse dye intermediate: adding a certain amount of acid into the mixed solution obtained in the step two, and fully stirring to uniformly mix the mixed solution;
step four: heating reaction of the disperse dye intermediate: fully reacting the mixed solution obtained in the third step at different temperatures;
step five: distillation of the disperse dye intermediate: distilling the mixed solution after the reaction in the fourth step;
step six: cooling treatment: cooling the disperse dye intermediate obtained in the fifth step to restore the temperature of the disperse dye intermediate to a normal temperature state;
step seven: addition of auxiliary agents: and adding a dispersing agent and a bactericide into the disperse dye intermediate recovered to the normal temperature, fully stirring and filtering.
Wherein:
and the filtering treatment in the first step is to adopt a multilayer filter to carry out precise filtration on the disperse dye intermediate to remove impurities in the disperse dye intermediate.
And the mass ratio of the water added in the second step to the disperse dye intermediate is 1: 30.
The mass ratio of the acid added in the third step to the disperse dye intermediate is 1: 4.
The temperature range in the fourth step is 90 ℃, and the reaction time is 3 hours.
And the dispersant in the seventh step is a mixture of polypropylene dilute hydrochloric acid and polymethyl methacrylate dilute hydrochloric acid, and the bactericide is sodium benzoate.
Example four
A green environment-friendly disperse dye intermediate treatment method comprises the following steps:
the method comprises the following steps: pretreatment of the environment-friendly disperse dye intermediate: filtering the environment-friendly disperse dye intermediate to remove impurities in the disperse dye intermediate;
step two: adding water to disperse dye intermediate: adding a certain amount of water into the intermediate of the disperse dye, and fully stirring;
step three: acid addition treatment of the disperse dye intermediate: adding a certain amount of acid into the mixed solution obtained in the step two, and fully stirring to uniformly mix the mixed solution;
step four: heating reaction of the disperse dye intermediate: fully reacting the mixed solution obtained in the third step at different temperatures;
step five: distillation of the disperse dye intermediate: distilling the mixed solution after the reaction in the fourth step;
step six: cooling treatment: cooling the disperse dye intermediate obtained in the fifth step to restore the temperature of the disperse dye intermediate to a normal temperature state;
step seven: addition of auxiliary agents: and adding a dispersing agent and a bactericide into the disperse dye intermediate recovered to the normal temperature, fully stirring and filtering.
Wherein:
and the filtering treatment in the first step is to adopt a multilayer filter to carry out precise filtration on the disperse dye intermediate to remove impurities in the disperse dye intermediate.
And the mass ratio of the water added in the second step to the disperse dye intermediate is 1: 35.
The mass ratio of the acid added in the third step to the disperse dye intermediate is 1: 5.
The different temperature conditions in the fourth step are 100 ℃, and the reaction time is 4 hours.
And the dispersant in the seventh step is a mixture of polypropylene dilute hydrochloric acid and polymethyl methacrylate dilute hydrochloric acid, and the bactericide is sodium benzoate.
EXAMPLE five
A green environment-friendly disperse dye intermediate treatment method comprises the following steps:
the method comprises the following steps: pretreatment of the environment-friendly disperse dye intermediate: filtering the environment-friendly disperse dye intermediate to remove impurities in the disperse dye intermediate;
step two: adding water to disperse dye intermediate: adding a certain amount of water into the intermediate of the disperse dye, and fully stirring;
step three: acid addition treatment of the disperse dye intermediate: adding a certain amount of acid into the mixed solution obtained in the step two, and fully stirring to uniformly mix the mixed solution;
step four: heating reaction of the disperse dye intermediate: fully reacting the mixed solution obtained in the third step at different temperatures;
step five: distillation of the disperse dye intermediate: distilling the mixed solution after the reaction in the fourth step;
step six: cooling treatment: cooling the disperse dye intermediate obtained in the fifth step to restore the temperature of the disperse dye intermediate to a normal temperature state;
step seven: addition of auxiliary agents: and adding a dispersing agent and a bactericide into the disperse dye intermediate recovered to the normal temperature, fully stirring and filtering.
Wherein:
and the filtering treatment in the first step is to adopt a multilayer filter to carry out precise filtration on the disperse dye intermediate to remove impurities in the disperse dye intermediate.
And the mass ratio of the water added in the second step to the disperse dye intermediate is 1: 40.
The mass ratio of the acid added in the third step to the disperse dye intermediate is 1: 6.5.
The temperature range of the different steps in the fourth step is 120 ℃, and the reaction time is 5.5 hours.
And the dispersant in the seventh step is a mixture of polypropylene dilute hydrochloric acid and polymethyl methacrylate dilute hydrochloric acid, and the bactericide is sodium benzoate.
EXAMPLE six
A green environment-friendly disperse dye intermediate treatment method comprises the following steps:
the method comprises the following steps: pretreatment of the environment-friendly disperse dye intermediate: filtering the environment-friendly disperse dye intermediate to remove impurities in the disperse dye intermediate;
step two: adding water to disperse dye intermediate: adding a certain amount of water into the intermediate of the disperse dye, and fully stirring;
step three: acid addition treatment of the disperse dye intermediate: adding a certain amount of acid into the mixed solution obtained in the step two, and fully stirring to uniformly mix the mixed solution;
step four: heating reaction of the disperse dye intermediate: fully reacting the mixed solution obtained in the third step at different temperatures;
step five: distillation of the disperse dye intermediate: distilling the mixed solution after the reaction in the fourth step;
step six: cooling treatment: cooling the disperse dye intermediate obtained in the fifth step to restore the temperature of the disperse dye intermediate to a normal temperature state;
step seven: addition of auxiliary agents: and adding a dispersing agent and a bactericide into the disperse dye intermediate recovered to the normal temperature, fully stirring and filtering.
Wherein:
and the filtering treatment in the first step is to adopt a multilayer filter to carry out precise filtration on the disperse dye intermediate to remove impurities in the disperse dye intermediate.
And the mass ratio of the water added in the second step to the disperse dye intermediate is 1: 45.
The mass ratio of the acid added in the third step to the disperse dye intermediate is 1: 8.
The temperature range in the fourth step is 135 ℃, and the reaction time is 7 hours.
And the dispersant in the seventh step is a mixture of polypropylene dilute hydrochloric acid and polymethyl methacrylate dilute hydrochloric acid, and the bactericide is sodium benzoate.
Through the above six groups of examples, the following data parameters were obtained
The test is carried out under the same condition, and the test table data shows that the treatment method of the disperse dye intermediate has obvious effect on reducing the content of chlorobenzene and chlorotoluene, and can more effectively reduce the content of chlorobenzene and chlorotoluene in the disperse dye intermediate along with the increase of water quantity and acid quantity, and the increase of reaction temperature and reaction time.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for processing an intermediate of a green environment-friendly disperse dye is characterized by comprising the following steps:
the method comprises the following steps: pretreatment of the environment-friendly disperse dye intermediate: filtering the environment-friendly disperse dye intermediate to remove impurities in the disperse dye intermediate;
step two: adding water to disperse dye intermediate: adding a certain amount of water into the intermediate of the disperse dye, and fully stirring;
step three: acid addition treatment of the disperse dye intermediate: adding a certain amount of acid into the mixed solution obtained in the step two, and fully stirring to uniformly mix the mixed solution;
step four: heating reaction of the disperse dye intermediate: fully reacting the mixed solution obtained in the third step at different temperatures;
step five: distillation of the disperse dye intermediate: distilling the mixed solution after the reaction in the fourth step;
step six: cooling treatment: cooling the disperse dye intermediate obtained in the fifth step to restore the temperature of the disperse dye intermediate to a normal temperature state;
step seven: addition of auxiliary agents: and adding a dispersing agent and a bactericide into the disperse dye intermediate recovered to the normal temperature, fully stirring and filtering.
2. The method for processing the green environment-friendly disperse dye intermediate according to claim 1, characterized in that: and the filtering treatment in the first step is to adopt a multilayer filter to carry out precise filtration on the disperse dye intermediate to remove impurities in the disperse dye intermediate.
3. The method for processing the green environment-friendly disperse dye intermediate according to claim 1, characterized in that: the mass ratio of the water added in the second step to the disperse dye intermediate is 1: 10-45.
4. The method for processing the green environment-friendly disperse dye intermediate according to claim 1, characterized in that: the mass ratio of the acid added in the third step to the disperse dye intermediate is 1: 2-8.
5. The method for processing the green environment-friendly disperse dye intermediate according to claim 1, characterized in that: the temperature range of the different temperature conditions in the fourth step is 70-135 ℃, and the reaction time is 2.5-7 hours.
6. The method for processing the green environment-friendly disperse dye intermediate according to claim 1, characterized in that: the dispersant in the seventh step is one or both of polypropylene dilute hydrochloric acid and polymethyl methacrylate dilute hydrochloric acid, and the bactericide is sodium benzoate.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725897A (en) * | 2013-12-23 | 2015-06-24 | 浙江龙盛集团股份有限公司 | Ecological environment-friendly treatment method of dye or dye intermediate |
| CN106748810A (en) * | 2016-12-30 | 2017-05-31 | 浙江闰土研究院有限公司 | A kind of processing method of disperse dyes intermediate |
| CN113527909A (en) * | 2021-07-23 | 2021-10-22 | 杭州吉华江东化工有限公司 | Synthesis process of environment-friendly dye |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725897A (en) * | 2013-12-23 | 2015-06-24 | 浙江龙盛集团股份有限公司 | Ecological environment-friendly treatment method of dye or dye intermediate |
| CN106748810A (en) * | 2016-12-30 | 2017-05-31 | 浙江闰土研究院有限公司 | A kind of processing method of disperse dyes intermediate |
| CN113527909A (en) * | 2021-07-23 | 2021-10-22 | 杭州吉华江东化工有限公司 | Synthesis process of environment-friendly dye |
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