CN106046916A - Preparation method of gel pen ink cleanser - Google Patents

Abstract

The invention discloses a preparation method of a neutral pen ink cleaner and belongs to the technical field of cleaner preparation. In the present invention, pomelo peels are made into powdered petroleum ether, stirred and heated, and the filtrate is evaporated after filtration to obtain pomelo peel crude oil, and the crude oil and absolute ethanol are stirred and evaporated to make pomelo peel refined oil, and the refined oil is used as a raw material to prepare epoxy resin Stir and heat pomelo oil and ethyl acetate, then add tin tetrachloride ethyl acetate solution to heat, filter and evaporate the filtrate to obtain polymerized epoxy pomelo oil, add it in an oil bath with potassium hydroxide solution, and then evaporate to dryness , collect dry crystalline ethyl acetate and stir and filter, adjust the pH of the filtrate, evaporate and collect the dry concentrate, and adjust the pH again to prepare a neutral pen ink cleaner. The preparation process of the present invention is simple, easy to use, and has excellent detergency Super strong, it can effectively remove the ink in the fine parts of the clothes without causing any damage to the clothes or the human body, and the cleaning speed of the cleaning agent is fast, which has great market promotion value.

Description

A kind of preparation method of neutral pen ink cleaning agent

technical field

The invention discloses a preparation method of a neutral pen ink cleaner and belongs to the technical field of cleaner preparation.

Background technique

The ballpoint pen with the viscosity of the writing medium between water and oil is called a gel pen. The gel pen originated in Japan. In 1988, the Japanese PENTEL Co., Ltd. successfully developed a product called "HYBRID", and the gel pen was born. . Because the gel pen has the advantages of both the fountain pen and the ballpoint pen, and has a comfortable writing feel, it is very popular among people and is a novel writing tool that is currently popular in the world.

There is an organic solvent inside the gel pen. Its viscosity is lower than that of oil-based ink and thicker than that of water-based ink. When writing, the ink passes through the nib, and it will change from semi-solid to liquid ink. The biggest advantage of gel pen ink is that every drop The ink is all used on the nib, which will not evaporate or leak, so it can provide a silky smooth writing feeling, and the ink flow is smooth and stable.

In daily work and study, gel pens have gradually become an indispensable part. However, many people have experienced this during use. Fingers, clothing, desktops, etc. found to be difficult to clean, so ink cleaners are playing an increasing role in cleaning ink problems.

However, due to the strong adhesion and cohesiveness of the ink, the existing ink cleaners are not ideal for cleaning the ink. The cleaning time is long, and long-term use will cause certain damage to the skin and clothing, seriously disturbing and affecting the normal work of workers.

Contents of the invention

The technical problem mainly solved by the present invention is that the current existing ink cleaners have poor cleaning effect, and it is difficult to clean the ink that penetrates into the clothes or embedded in the palm prints, nail crevices, etc., and the cleaning time is too long. Long-term use will cause certain damage to the skin and clothing. A preparation method for gel pen ink cleaner is provided. In this method, pomelo peel is made into powdered petroleum ether, stirred and heated, and the filtrate is evaporated after filtration to obtain pomelo peel crude oil. , stirring and evaporating the crude oil with absolute ethanol to make pomelo peel refined oil, and stirring and heating the epoxy pomelo peel oil and ethyl acetate prepared from the pomelo peel refined oil as raw materials, then adding tin tetrachloride ethyl acetate solution to heat, Filtrate and evaporate the filtrate to obtain polymerized epoxy pomelo oil, add it and potassium hydroxide solution in an oil bath, then evaporate to dryness, collect dry crystalline ethyl acetate, stir and filter, adjust the pH of the filtrate, and evaporate to collect the dry concentrate. After adjusting the pH again, a neutral pen ink cleaner can be prepared. The preparation process of the present invention is simple, easy to use, and has super detergency, which can effectively remove ink from clothing, skin and subtle places without damaging clothing or human body. No damage is caused, and the cleaning speed of the cleaning agent is very fast, which is of great marketing value.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:

(1) Select fresh pomelo peel, dry it at 65-70°C for 6-8 hours, then let it stand to cool to room temperature, grind and pass through a 75-80 mesh sieve, collect pomelo peel powder, and use a mass ratio of 1:15 , Stir and mix pomelo peel powder and petroleum ether, and heat in a water bath at 35-40°C for 85-90 minutes;

(2) After the heating in the water bath is completed, filter and collect the filtrate, and rotary evaporate at 65-70°C to 1/5 of the original volume to prepare the crude pomelo peel oil, and then mix the pomelo peel crude oil with a volume ratio of 1:5 Stirring and mixing with absolute ethanol, and rotary evaporation at 45-50°C to 1/6 of the original volume to prepare pomelo peel refined oil;

(3) Select 150-160mL of the pomelo peel refined oil prepared above and place it in a three-necked flask, heat it in a water bath at 65-70°C for 25-30min, then select 45-48mL of 10% hydrogen peroxide solution with a mass concentration of 10% and drop it into the three-necked flask. Control the dropping time for 1.5-2.0 hours. After the dropping is completed, heat it at 65-70°C for 6-8 hours, then stop heating and let it stand for stratification. Collect the oil layer and rotary evaporate to 1/3 of the original volume. Prepared epoxy pomelo oil;

(4) Select 45-50mL of the above-prepared epoxy pomelo oil and 65-70mL of ethyl acetate in a three-necked flask, stir and mix, and heat in a water bath at 45-60°C for 25-30min. After the water bath heating is completed, Add 4.5 to 4.6 g of tin tetrachloride ethyl acetate solution with a mass concentration of 1% to the three-necked flask dropwise, and control the dropping time to 100 to 120 minutes;

(5) After the dropwise addition is completed, keep warm and heat for 1-2 hours, then stop heating and let it stand to cool to room temperature, filter and collect the filtrate, collect the filtrate and place it at 65-70°C for rotary evaporation to 1/3 of the original volume, Prepared polymerized epoxy pomelo oil;

(6) Select 5.0-5.2g of the above-prepared polymerized epoxy pomelo oil and 152-155mL of potassium hydroxide solution with a concentration of 1mol/L in a beaker, heat in an oil bath at 100-105°C for 6-8 hours, and then stop Heating, rotary evaporation at 65-70°C to dryness, collecting dry crystals;

(7) Stir and mix the dried crystals prepared above with ethyl acetate at a mass ratio of 1:10, then filter and collect the filtrate, adjust the pH to 6.0 with a 10% hydrochloric acid solution, and evaporate at 65-70°C to 1/10 of the original volume, collect the dried concentrated solution, and adjust the pH to 9.0 with a 10% potassium hydroxide solution to prepare a neutral pen ink cleaner.

The use method of the present invention is: mix the neutral pen ink cleanser prepared by the present invention with 0.5-1.0% of warm water mass into warm water, then stir the water and the cleanser evenly, soak the clothes in water for 3-5 minutes, then Gently scrub the clothes clean. After testing, the cleaning rate of the ink cleaner prepared by the invention can reach 96-99%, the cleaning ability is good, and the clothes will not be damaged, and the cleaning speed is 2-4 times higher than that of ordinary ink cleaners.

The beneficial effects of the present invention are:

(1) The preparation process of the present invention is simple and easy to use, and the prepared gel pen ink cleaner has super decontamination ability, fast cleaning speed, and effectively improves the cleaning efficiency;

(2) The gel pen ink cleaner prepared by the present invention can effectively remove the ink penetrating into the fine parts of clothes and skin without causing any damage to clothes and skin.

detailed description

First select fresh pomelo peels, dry them at 65-70°C for 6-8 hours, then let them cool down to room temperature, grind them and pass through a 75-80 mesh sieve to collect pomelo peel powder, and mix them in a mass ratio of 1:15. Stir and mix pomelo peel powder and petroleum ether, heat in a water bath at 35-40°C for 85-90 minutes; after the heating in a water bath is completed, filter and collect the filtrate, and rotary evaporate at 65-70°C to 1/5 of the original volume to prepare Crude pomelo peel oil, followed by stirring and mixing the crude pomelo peel oil with absolute ethanol at a volume ratio of 1:5, and rotary evaporation at 45-50°C to 1/6 of the original volume to prepare pomelo peel refined oil; then select Put 150-160mL of the pomelo peel refined oil prepared above in a three-necked flask, heat it in a water bath at 65-70°C for 25-30 minutes, then select 45-48mL of 10% hydrogen peroxide solution with a mass concentration of 10% and drop it into the three-necked flask, and control the dropping time 1.5~2.0h. After the dropwise addition is completed, heat it at 65~70°C for 6~8h, then stop heating and let it stand for stratification. Collect the oil layer and rotary evaporate to 1/3 of the original volume to prepare epoxy resin Pomelo oil; then select 45-50mL of the above-prepared epoxy pomelo oil and 65-70mL of ethyl acetate in a three-necked flask, stir and mix them and place them in a water bath at 45-60°C for 25-30 minutes until the water bath heating is complete Finally, add 4.5 to 4.6 g of tin tetrachloride ethyl acetate solution with a mass concentration of 1% to the three-necked flask dropwise, and control the dropping time to 100 to 120 minutes; Stand to cool to room temperature, filter and collect the filtrate, collect the filtrate and place it at 65-70°C for rotary evaporation to 1/3 of the original volume to prepare polymerized epoxy pomelo oil; then select 5.0-5.2g of the above-prepared ring Pomelo oil and 152-155 mL of potassium hydroxide solution with a concentration of 1 mol/L were placed in a beaker, heated in an oil bath at 100-105°C for 6-8 hours, then stopped heating, and evaporated to dryness at 65-70°C. Collect dry crystals; finally, according to the mass ratio of 1:10, stir and mix the dry crystals prepared above with ethyl acetate, then filter and collect the filtrate, adjust the pH to 6.0 with 10% hydrochloric acid solution, and rotate at 65-70°C Evaporate to 1/10 of the original volume, collect the dried concentrate, and adjust the pH to 9.0 with a mass concentration of 10% potassium hydroxide solution to prepare a neutral pen ink cleaner.

Example 1

First select fresh pomelo peel, dry it at 65°C for 6 hours, then let it stand to cool to room temperature, grind and pass through a 75-mesh sieve to collect grapefruit peel powder, and mix grapefruit peel powder with petroleum ether at a mass ratio of 1:15 Stir and mix, and heat in a water bath at 35°C for 85 minutes; after the water bath heating is completed, filter and collect the filtrate, and rotary evaporate at 65°C to 1/5 of the original volume to prepare pomelo peel crude oil, which is then mixed at a volume ratio of 1:5 , stir and mix the crude pomelo peel oil with absolute ethanol, and rotary evaporate at 45°C to 1/6 of the original volume to prepare refined pomelo peel oil; then select 150mL of the above-mentioned refined pomelo peel oil and place it in a three-necked flask, Heated in a water bath at 65°C for 25 minutes, then selected 45mL of 10% hydrogen peroxide solution and added it dropwise to a three-necked flask, and controlled the dropping time for 1.5h. Stand to separate layers, collect the oil layer and rotary evaporate to 1/3 of the original volume to prepare epoxy pomelo oil; then select 45mL epoxy pomelo oil prepared above and 65mL ethyl acetate in a three-necked flask, stir and mix And place it in a water bath at 45°C for 25 minutes. After the water bath heating is completed, add 4.5 g of tin tetrachloride ethyl acetate solution with a mass concentration of 1% to the three-necked flask dropwise, and control the dropping time to 100 minutes; after the dropwise addition is completed, Insulate and heat for 1 hour, then stop heating and let stand to cool to room temperature, filter and collect the filtrate, collect the filtrate and place it at 65°C for rotary evaporation to 1/3 of the original volume to prepare polymerized epoxy pomelo oil; then select 5.0g The above-prepared epoxy pomelo oil and 152 mL of potassium hydroxide solution with a concentration of 1 mol/L were placed in a beaker, heated in an oil bath at 100°C for 6 hours, then the heating was stopped, and the dry crystals were collected by rotary evaporation at 65°C; Finally, according to the mass ratio of 1:10, the dry crystals prepared above were stirred and mixed with ethyl acetate, then filtered and the filtrate was collected, and the pH was adjusted to 6.0 with 10% hydrochloric acid solution with a mass concentration, and rotary evaporated at 65°C to 1% of the original volume. /10, collect the dry concentrate, and adjust the pH to 9.0 with a mass concentration of 10% potassium hydroxide solution to prepare a neutral pen ink cleaner.

This example is easy to operate, and when in use, the neutral pen ink cleaner prepared by the present invention with 0.5% of warm water quality is mixed into warm water, then the water and the cleaner are stirred evenly, the clothes are soaked in water for 3min, and then the clothes are lightly Scrub lightly to clean. After testing, the ink cleaning agent prepared by the invention has a cleaning rate of up to 96%, good cleaning ability, no damage to clothes, and the cleaning speed is twice as high as that of ordinary ink cleaning agents.

Example 2

First select fresh pomelo peel, dry it at 68°C for 7 hours, then let it stand to cool to room temperature, grind and pass through a 78-mesh sieve to collect grapefruit peel powder, and mix grapefruit peel powder with petroleum ether at a mass ratio of 1:15 Stir and mix, and heat in a water bath at 38°C for 88 minutes; after the water bath heating is completed, filter and collect the filtrate, and rotary evaporate at 68°C to 1/5 of the original volume to prepare pomelo peel crude oil, which is then mixed at a volume ratio of 1:5 , stirring and mixing the crude pomelo peel oil with absolute ethanol, and rotary evaporating at 48°C to 1/6 of the original volume to prepare refined pomelo peel oil; then select 155mL of the above-mentioned refined pomelo peel oil and place it in a three-necked flask, Heated in a water bath at 68°C for 28 minutes, then selected 47mL of 10% hydrogen peroxide solution and added it dropwise to a three-necked flask, and controlled the dropping time for 1.8h. Stand to separate layers, collect the oil layer and rotary evaporate to 1/3 of the original volume to prepare epoxy pomelo oil; then select 48mL epoxy pomelo oil prepared above and 68mL ethyl acetate in a three-necked flask, stir and mix And place it in a water bath at 53°C for 28 minutes. After the water bath heating is completed, add 4.55 g of tin tetrachloride ethyl acetate solution with a mass concentration of 1% to the three-necked flask dropwise, and control the dropping time to 110 minutes; after the dropwise addition is completed, Insulate and heat for 1.5h, then stop heating and let stand to cool to room temperature, filter and collect the filtrate, collect the filtrate and place it at 68°C for rotary evaporation to 1/3 of the original volume to prepare polymerized epoxy pomelo peel oil; then select 5.1 g Epoxy pomelo oil prepared above and 154 mL of potassium hydroxide solution with a concentration of 1 mol/L were placed in a beaker, heated in an oil bath at 103°C for 7 hours, then the heating was stopped, and the dry crystals were collected by rotary evaporation at 68°C ; Finally, according to the mass ratio of 1:10, the dry crystals prepared above were stirred and mixed with ethyl acetate, then filtered and the filtrate was collected, and the pH was adjusted to 6.0 with a mass concentration of 10% hydrochloric acid solution, and then rotary evaporated to the original volume at 68°C 1/10, collect the dried concentrated solution, and adjust the pH to 9.0 with a mass concentration of 10% potassium hydroxide solution to prepare a neutral pen ink cleaner.

This example is easy to operate, and when in use, the neutral pen ink cleaner prepared by the present invention with a warm water quality of 0.8% is mixed into warm water, then the water and the cleaner are stirred evenly, the clothes are soaked in water for 4min, and then the clothes are lightly Scrub lightly to clean. After testing, the ink cleaning agent prepared by the invention has a cleaning rate of up to 98%, has good cleaning ability, does not cause damage to clothes, and has a cleaning speed three times higher than that of ordinary ink cleaning agents.

Example 3

First select fresh pomelo peels, dry them at 70°C for 8 hours, then let them stand to cool to room temperature, grind them and pass them through an 80-mesh sieve to collect pomelo peel powders, mix the grapefruit peel powders with petroleum ether at a mass ratio of 1:15 Stir and mix, and heat in a water bath at 40°C for 90 minutes; after the water bath heating is completed, filter and collect the filtrate, and rotary evaporate at 70°C to 1/5 of the original volume to prepare pomelo peel crude oil, which is then mixed at a volume ratio of 1:5 , stirring and mixing the crude pomelo peel oil with absolute ethanol, and rotary evaporating at 50°C to 1/6 of the original volume to prepare refined pomelo peel oil; then select 160mL of the above-mentioned refined pomelo peel oil and place it in a three-necked flask, Heated in a water bath at 70°C for 30min, then selected 48mL of 10% hydrogen peroxide solution and added it dropwise to a three-necked flask, and controlled the dropping time for 2.0h. Stand to separate layers, collect the oil layer and rotary evaporate to 1/3 of the original volume to prepare epoxy pomelo oil; then select 50mL epoxy pomelo oil prepared above and 70mL ethyl acetate in a three-necked flask, stir and mix And place it in a water bath at 60°C for 30 minutes. After the water bath heating is completed, add 4.6 g of tin tetrachloride ethyl acetate solution with a mass concentration of 1% to the three-necked flask dropwise, and control the dropping time to 120 minutes; after the dropwise addition is completed, Insulate and heat for 2 hours, then stop heating and let stand to cool to room temperature, filter and collect the filtrate, collect the filtrate and place it at 70°C for rotary evaporation to 1/3 of the original volume to prepare polymerized epoxy pomelo oil; then select 5.2g The epoxy pomelo oil prepared above and 155 mL of potassium hydroxide solution with a concentration of 1 mol/L were placed in a beaker, heated in an oil bath at 105°C for 8 hours, then the heating was stopped, and the dry crystals were collected by rotary evaporation at 70°C; Finally, according to the mass ratio of 1:10, the dry crystals prepared above were stirred and mixed with ethyl acetate, then filtered and the filtrate was collected, and the pH was adjusted to 6.0 with 10% hydrochloric acid solution with a mass concentration of 1, and then rotary evaporated at 70°C to 1% of the original volume. /10, collect the dry concentrate, and adjust the pH to 9.0 with a mass concentration of 10% potassium hydroxide solution to prepare a neutral pen ink cleaner.

This example is easy to operate, and when in use, the neutral pen ink cleaner prepared by the present invention with 1.0% of the warm water quality is mixed into warm water, then the water and the cleaner are stirred evenly, the clothes are soaked in water for 5 minutes, and then the clothes are lightly washed Scrub lightly to clean. After testing, the cleaning rate of the ink cleaner prepared by the invention can reach 99%, the cleaning ability is good, and the clothes will not be damaged, and the cleaning speed is 4 times higher than that of ordinary ink cleaners.

Claims (1)

1. a preparation method of neutral pen ink cleaner, is characterized in that concrete preparation steps are: (1) Select fresh pomelo peel, dry it at 65-70°C for 6-8 hours, then let it stand to cool to room temperature, grind and pass through a 75-80 mesh sieve, collect pomelo peel powder, and use a mass ratio of 1:15 , Stir and mix pomelo peel powder and petroleum ether, and heat in a water bath at 35-40°C for 85-90 minutes; (2) After the heating in the water bath is completed, filter and collect the filtrate, and rotary evaporate at 65-70°C to 1/5 of the original volume to prepare the crude pomelo peel oil, and then mix the pomelo peel crude oil with a volume ratio of 1:5 Stirring and mixing with absolute ethanol, and rotary evaporation at 45-50°C to 1/6 of the original volume to prepare pomelo peel refined oil; (3) Select 150-160mL of the pomelo peel refined oil prepared above and place it in a three-necked flask, heat it in a water bath at 65-70°C for 25-30min, then select 45-48mL of 10% hydrogen peroxide solution with a mass concentration of 10% and drop it into the three-necked flask. Control the dropping time for 1.5-2.0 hours. After the dropping is completed, heat it at 65-70°C for 6-8 hours, then stop heating and let it stand for stratification. Collect the oil layer and rotary evaporate to 1/3 of the original volume. Prepared epoxy pomelo oil; (4) Select 45-50mL of the above-prepared polymerized epoxy pomelo oil and 65-70mL of ethyl acetate in a three-necked flask, stir and mix, and heat in a water bath at 45-60°C for 25-30min. After the water bath heating is completed , add 4.5 to 4.6 g of tin tetrachloride ethyl acetate solution with a mass concentration of 1% to the three-necked flask dropwise, and control the dropping time to 100 to 120 minutes; (5) After the dropwise addition is completed, keep warm and heat for 1-2 hours, then stop heating and let it stand to cool to room temperature, filter and collect the filtrate, collect the filtrate and place it at 65-70°C for rotary evaporation to 1/3 of the original volume, Prepared polymerized epoxy pomelo oil; (6) Select 5.0-5.2g of epoxy pomelo oil prepared above and 152-155mL of potassium hydroxide solution with a concentration of 1mol/L in a beaker, heat in an oil bath at 100-105°C for 6-8h, then stop heating , rotary evaporated to dryness at 65-70°C, and collected dried crystals; (7) Stir and mix the dried crystals prepared above with ethyl acetate at a mass ratio of 1:10, then filter and collect the filtrate, adjust the pH to 6.0 with a 10% hydrochloric acid solution, and evaporate at 65-70°C to 1/10 of the original volume, collect the dried concentrated solution, and adjust the pH to 9.0 with a 10% potassium hydroxide solution to prepare a neutral pen ink cleaner.