阅读说明：本技术 一种利用生产没食子酸的废水生产蓝黑墨水的方法 (Method for producing blue black ink by using wastewater from gallic acid production ) 是由 蒋黎明 于 2019-12-02 设计创作，主要内容包括：本申请公开了一种利用生产没食子酸的废水生产蓝黑墨水的方法,包括以下步骤：生产没食子酸的废水,加入氢氧化钙悬浊液,第一混匀,第一静置,过滤,得到滤液；搅拌下向硫酸亚铁中加入过氧化氢溶液,反应生成混合液；所述滤液加入到所述混合液中,第二混匀,第二静置,得到水性染料；水性染料加入丙三醇、分散剂,并可选的加入香精,第三混匀,制得蓝黑墨水。本申请提供的方法,工艺简单、生产周期短,能将生产没食子酸的废水制备成蓝黑墨水,变废为宝,既有利于废水的处理,又可大幅降低制备墨水的原料价格,降低成本；所制备的蓝黑墨水,尤其适合用于写毛笔字。(The application discloses a method for producing blue-black ink by using wastewater from gallic acid production, which comprises the following steps: adding calcium hydroxide suspension into wastewater from gallic acid production, mixing, standing, and filtering to obtain filtrate; adding a hydrogen peroxide solution into ferrous sulfate under stirring to react to generate a mixed solution; adding the filtrate into the mixed solution, uniformly mixing the filtrate and the mixed solution for the second time, and standing the mixture for the second time to obtain the water-based dye; and adding glycerol and a dispersing agent into the water-based dye, optionally adding essence, and uniformly mixing to obtain the blue-black ink. The method provided by the application has the advantages of simple process and short production period, can prepare the wastewater for producing the gallic acid into the blue-black ink, changes waste into valuable, is beneficial to the treatment of the wastewater, and can greatly reduce the price of raw materials for preparing the ink and reduce the cost; the prepared blue-black ink is especially suitable for writing brush characters.)

1. A method for producing blue black ink by using wastewater from gallic acid production is characterized by comprising the following steps:

adding calcium hydroxide suspension into wastewater from gallic acid production, mixing, standing, and filtering to obtain filtrate;

adding a hydrogen peroxide solution into ferrous sulfate under stirring to react to generate a mixed solution;

adding the filtrate into the mixed solution, uniformly mixing the filtrate and the mixed solution for the second time, and standing the mixture for the second time to obtain the water-based dye;

and adding glycerol and a dispersing agent into the water-based dye, optionally adding essence, and uniformly mixing to obtain the blue-black ink.

2. The method according to claim 1, wherein the calcium hydroxide is used in an amount of 6.5 to 7.5kg per 100kg of wastewater.

3. The method according to claim 1, wherein the first resting time is 2-5 h; and/or the presence of a gas in the gas,

the filtration comprises rough filtration and fine filtration, wherein a screen with 350 meshes and 400 meshes is used for the rough filtration, and a polymer filter membrane with the diameter of 1-1.5 mu m is used for the fine filtration.

4. The method according to claim 3, wherein the screen is in particular a filter cloth and the polymeric filter membrane is in particular PP cotton.

5. The method according to claim 1, wherein the hydrogen peroxide solution has a concentration of 30-35% by mass, and the ratio of the ferrous sulfate to the hydrogen peroxide solution is: using 18-25kg of hydrogen peroxide solution for 7.5-10.5kg of ferrous sulfate, and reacting to generate mixed liquor.

6. The method of claim 5, wherein the ratio of the filtrate to the mixed liquor is: 7.5-10.5kg of ferrous sulfate and 18-25kg of hydrogen peroxide solution, and adding 150-155L of the filtrate.

7. The method of claim 1, wherein the second resting time is 10-15 min.

8. The process according to claim 1, characterized in that the dispersant is in particular dispersant 5040.

9. The method according to claim 1, wherein the amount of each substance is, in weight percent: the amount of the glycerol is 0.5-3% of that of the water-based dye, the amount of the dispersing agent is 0.2-2% of that of the water-based dye, and the amount of the essence is 0.1-0.2 per mill of that of the water-based dye.

10. The method of claim 1, further comprising the steps of filling, packaging and packaging the blue-black ink to obtain a finished product.

Technical Field

The application relates to the technical field of daily chemical product production, in particular to a method for producing blue-black ink by using wastewater generated in gallic acid production.

Background

The gallic acid extracted from gallnut and tara powder can generate a large amount of mother liquor containing tannic acid and gallic acid, the mother liquor can only be used for treating wastewater generally, and because the COD concentration in the mother liquor is higher, the tannic acid and the gallic acid have the bactericidal effect, so that the cost for treating the wastewater is very high. The construction of a sewage treatment plant for treating 25 tons of mother liquor per day requires 1000 ten thousand investment and also requires 120-150 ten thousand operation cost each year. In order to improve the efficiency of enterprises and develop green chemistry, the treatment cost of mother liquor needs to be reduced or the mother liquor needs to be recycled to change waste into valuable.

Disclosure of Invention

In order to solve the above technical problems, a first object of the present invention is to provide a method for producing blue-black ink using wastewater from gallic acid production; the method provided by the application has the advantages of simple process and short production period, can prepare the wastewater for producing the gallic acid into the blue-black ink, changes waste into valuable, is beneficial to the treatment of the wastewater, and can greatly reduce the price of raw materials for preparing the ink and reduce the cost; the prepared blue-black ink is especially suitable for writing brush characters.

The technical scheme provided by the invention is as follows:

a method for producing blue black ink by using wastewater from gallic acid production comprises the following steps:

adding calcium hydroxide suspension into wastewater from gallic acid production, mixing, standing, and filtering to obtain filtrate;

adding a hydrogen peroxide solution into ferrous sulfate under stirring to react to generate a mixed solution;

adding the filtrate into the mixed solution, uniformly mixing the filtrate and the mixed solution for the second time, and standing the mixture for the second time to obtain the water-based dye;

and adding glycerol and a dispersing agent into the water-based dye, optionally adding essence, and uniformly mixing to obtain the blue-black ink.

Preferably, the amount of calcium hydroxide is 6.5-7.5kg per 100kg of wastewater.

Preferably, the first standing time is 2-5 h; and/or the presence of a gas in the gas,

the filtration comprises rough filtration and fine filtration, wherein a screen with 350 meshes and 400 meshes is used for the rough filtration, and a polymer filter membrane with the diameter of 1-1.5 mu m is used for the fine filtration.

Preferably, the screen is filter cloth, and the polymer filter membrane is PP cotton.

Preferably, the mass percentage concentration of the hydrogen peroxide solution is 30-35%, and the usage ratio of the ferrous sulfate to the hydrogen peroxide solution is as follows: using 18-25kg of hydrogen peroxide solution for 7.5-10.5kg of ferrous sulfate, and reacting to generate mixed liquor.

Preferably, the dosage ratio of the filtrate to the mixed solution is: 7.5-10.5kg of ferrous sulfate and 18-25kg of hydrogen peroxide solution, and adding 150-155L of the filtrate.

Preferably, the time of the second standing is 10-15 min.

Preferably, the dispersant is specifically dispersant 5040.

Preferably, the dosage of each substance is calculated by weight percentage as follows: the amount of the glycerol is 0.5-3% of that of the water-based dye, the amount of the dispersing agent is 0.2-2% of that of the water-based dye, and the amount of the essence is 0.1-0.2 per mill of that of the water-based dye.

Preferably, the method further comprises the steps of filling, packaging and packaging the blue-black ink to obtain a finished product.

The applicant detects the wastewater generated in the production of gallic acid from gallnut or tara powder, and finds that the main components of the wastewater comprise, by mass: 0.8-1.1% of glucose, 8-11% of sodium chloride, 0.4-1.0% of tannic acid, 0.5-1.3% of gallic acid, 0.4-0.6% of tannic acid, 1.3-1.6% of hydrochloric acid and the balance of water. The applicant has found that the gallic acid, tannic acid and other components contained in the wastewater are suitable for producing blue-black water-based dyes, and the blue-black ink can be prepared by adding glycerol and a dispersing agent. In order to meet the requirements of consumers, essence can also be added to provide aromatic odor.

The applicant finds that the mixed solution generated by adding the ferrous sulfate into the hydrogen peroxide solution for reaction can form a blue-black water-based dye with a darker color after reacting with the filtrate, and other dyes are not required to be additionally added for deepening the color of the ink. And due to the existence of the hydrogen peroxide, the generated aqueous dye is thick and does not contain precipitates, so that the pen cannot be blocked, and the use of the ink cannot be influenced. The applicant uses a ferrous sulfate solution (without adding hydrogen peroxide) and a ferric sulfate solution, and compares the ferrous sulfate solution and the ferric sulfate solution with the scheme adopted by the application, and the result shows that the ink prepared by solely using ferrous sulfate has insufficient color; and the ink prepared by singly using the ferric sulfate forms colloid after writing, has insufficient black color and precipitates, and influences the use of the ink.

The method provided by the application has the advantages of simple process and short production period, can prepare the wastewater for producing the gallic acid into the blue-black ink, changes waste into valuable, is beneficial to the treatment of the wastewater, and can greatly reduce the price of raw materials for preparing the ink and reduce the cost; the prepared blue-black ink is especially suitable for writing brush characters.

Detailed Description

In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present application, 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 application.

The embodiments of the present application are written in a progressive manner.

The embodiment of the invention provides a method for producing blue-black ink by using wastewater from gallic acid production, which comprises the following steps:

adding calcium hydroxide suspension into wastewater from gallic acid production, mixing, standing, and filtering to obtain filtrate;

adding a hydrogen peroxide solution into ferrous sulfate under stirring to react to generate a mixed solution;

adding the filtrate into the mixed solution, uniformly mixing the filtrate and the mixed solution for the second time, and standing the mixture for the second time to obtain the water-based dye;

and adding glycerol and a dispersing agent into the water-based dye, optionally adding essence, and uniformly mixing to obtain the blue-black ink.

The applicant detects the wastewater generated in the production of gallic acid from gallnut or tara powder, and finds that the main components of the wastewater comprise, by mass: 0.8-1.1% of glucose, 8-11% of sodium chloride, 0.4-1.0% of tannic acid, 0.5-1.3% of gallic acid, 0.4-0.6% of tannic acid, 1.3-1.6% of hydrochloric acid and the balance of water. The applicant has found that the gallic acid, tannic acid and other components contained in the wastewater are suitable for producing blue-black water-based dyes, and the blue-black ink can be prepared by adding glycerol and a dispersing agent. In order to meet the requirements of consumers, essence can also be added to provide aromatic odor.

The applicant finds that the mixed solution generated by adding the ferrous sulfate into the hydrogen peroxide solution for reaction can form a blue-black water-based dye with a darker color after reacting with the filtrate, and other dyes are not required to be additionally added for deepening the color of the ink. And due to the existence of the hydrogen peroxide, the generated aqueous dye is thick and does not contain precipitates, so that the pen cannot be blocked, and the use of the ink cannot be influenced. The applicant uses a ferrous sulfate solution (without adding hydrogen peroxide) and a ferric sulfate solution, and compares the ferrous sulfate solution and the ferric sulfate solution with the scheme adopted by the application, and the result shows that the ink prepared by solely using ferrous sulfate has insufficient color; and the ink prepared by singly using the ferric sulfate forms colloid after writing, has insufficient black color and precipitates, and influences the use of the ink.

The method provided by the application has the advantages of simple process and short production period, can prepare the wastewater for producing the gallic acid into the blue-black ink, changes waste into valuable, is beneficial to the treatment of the wastewater, and can greatly reduce the price of raw materials for preparing the ink and reduce the cost; the prepared blue-black ink is especially suitable for writing brush characters.

Preferably, the amount of calcium hydroxide is 6.5-7.5kg per 100kg of wastewater.

The calcium hydroxide suspension is used, and the weight ratio of the calcium hydroxide solid to the wastewater is controlled, so that the acidic components in the wastewater can be effectively neutralized, and the using amount of the calcium hydroxide is saved.

Preferably, the first standing time is 2-5 h; and/or the presence of a gas in the gas,

the filtration comprises rough filtration and fine filtration, wherein a screen with 350 meshes and 400 meshes is used for the rough filtration, and a polymer filter membrane with the diameter of 1-1.5 mu m is used for the fine filtration.

Preferably, the screen is filter cloth, and the polymer filter membrane is PP cotton.

The liquid after the reaction with the calcium hydroxide is kept stand, preferably for 2 to 5 hours, more preferably for 2 to 3 hours, so that solid matters can be precipitated, and the filtering operation is facilitated. The filtration is preferably carried out sequentially by coarse filtration and fine filtration, wherein the coarse filtration uses a 400-mesh screen with 350 meshes and preferably uses a 300-mesh filter cloth to filter larger particles in the liquid, the filtrate after the coarse filtration is further subjected to fine filtration, and the fine filtration uses a 1-1.5 mu m high molecular filter membrane, preferably PP cotton, for example, a 1 mu m PP cotton filter.

Preferably, the mass percentage concentration of the hydrogen peroxide solution is 30-35%, and the usage ratio of the ferrous sulfate to the hydrogen peroxide solution is as follows: using 18-25kg of hydrogen peroxide solution for 7.5-10.5kg of ferrous sulfate, and reacting to generate mixed liquor.

The hydrogen peroxide solution is preferably used in a concentration of 30 to 35% by mass, more preferably 30 to 32% by mass, and the solid ferrous sulfate is oxidized and dissolved by the heat generated by the reaction of the hydrogen peroxide and the ferrous sulfate. And adding the filtrate into the mixed solution while the solution is hot, preferably stirring and adding the filtrate, uniformly mixing the filtrate and the mixed solution for the second time (uniformly stirring), and standing the mixture for 10 to 15min, preferably standing the mixture for 10 to 15min to obtain the bluish black water-based dye.

Preferably, the dosage ratio of the filtrate to the mixed solution is: 7.5-10.5kg of ferrous sulfate and 18-25kg of hydrogen peroxide solution, and adding 150-155L of the filtrate.

Preferably, the time of the second standing is 10-15 min.

Preferably, the dispersant is specifically dispersant 5040.

Preferably, the dosage of each substance is calculated by weight percentage as follows: the amount of the glycerol is 0.5-3% of that of the water-based dye, the amount of the dispersing agent is 0.2-2% of that of the water-based dye, and the amount of the essence is 0.1-0.2 per mill of that of the water-based dye.

Preferably, the method further comprises the steps of filling, packaging and packaging the blue-black ink to obtain a finished product.

The prepared blue-black ink is preferably filled, more preferably filled into glass bottles, and then packaged and filled into packaging cartons to prepare finished products for sale.