CN115710443B - Degradable liquid chalk and preparation method thereof - Google Patents
Degradable liquid chalk and preparation method thereof Download PDFInfo
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- CN115710443B CN115710443B CN202211426864.0A CN202211426864A CN115710443B CN 115710443 B CN115710443 B CN 115710443B CN 202211426864 A CN202211426864 A CN 202211426864A CN 115710443 B CN115710443 B CN 115710443B
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Abstract
The invention discloses a degradable liquid chalk and a preparation method thereof, wherein the preparation raw materials comprise the following components in parts by weight: 8-20 parts of film-forming resin, 8-30 parts of titanium dioxide, 0-3 parts of water-based pigment, 0.5-4 parts of emulsifier, 1-3 parts of dispersing agent, 1-2 parts of stabilizer, 0.5-2 parts of flatting agent, 1-3 parts of humectant, 33-76 parts of deionized water and 30-50 parts of solvent. The chalk disclosed by the invention has the advantages of good writing feel, good cleaning effect, easiness in erasing after writing, good erasable effect on uneven writing surfaces, capability of degrading biological or other forms by film forming substances falling off after erasing, and capability of avoiding plastic pollution.
Description
Technical Field
The invention relates to the technical field of teaching stationery, relates to the field of C09D13/00, and in particular relates to a degradable liquid chalk and a preparation method thereof.
Background
Chalk is an important teaching tool, and can be frequently and largely used in the teaching process. The traditional chalk is mainly made of calcium sulfate, calcium carbonate and the like as main materials, and a large amount of dust is generated when the chalk is erased, so that the health of a user and surrounding people is endangered, and aiming at the problem, people invent a liquid chalk to reduce or avoid the problem of dust generated in the using process.
Film formers, which are important components of liquid chalks and have an important influence on their properties, are mostly polymer resins, which are used in the literature reported so far, because of their non-degradability, which, after being erased, are difficult to avoid, which causes certain problems of plastic contamination. For example, CN 101457055a discloses an aqueous liquid chalk, which uses polyvinyl butyral as a film forming agent, and has certain elasticity, but is not degradable, and is not easy to erase due to good adhesion.
CN102020892a discloses a method for preparing water-wiping teaching ink, in the invention, substances such as methyl cellulose, carboxymethyl cellulose and the like are taken as film forming agents, and although the film forming agents can be degraded in natural environment, the film forming agents have no elasticity, and the removal effect after writing is not ideal, so that the teaching ink obtained by the invention can be rewritten after being wiped with water after a blackboard is dried, and the efficiency is lower.
Disclosure of Invention
Aiming at the problems, the invention discloses a degradable liquid chalk, which comprises the following raw materials in parts by weight: 8-20 parts of film-forming resin, 8-30 parts of titanium dioxide, 0-3 parts of water-based pigment, 0.5-4 parts of emulsifier, 1-3 parts of dispersing agent, 1-2 parts of stabilizer, 0.5-2 parts of flatting agent, 1-3 parts of humectant, 33-76 parts of deionized water and 30-50 parts of solvent.
For example, the preparation raw materials comprise the following components in parts by weight: 10 parts of film-forming resin, 20 parts of titanium dioxide, 1.5 parts of emulsifier, 1.5 parts of dispersing agent, 1.5 parts of stabilizer, 1 part of leveling agent, 1 part of humectant, 63.5 parts of deionized water and 40 parts of solvent.
Such as: the preparation raw materials comprise the following components in parts by weight: 15 parts of film-forming resin, 10 parts of titanium dioxide, 2 parts of water-based pigment, 2 parts of emulsifier, 1 part of dispersing agent, 1 part of stabilizer, 1 part of leveling agent, 1 part of humectant, 67 parts of deionized water and 45 parts of solvent.
In one embodiment, the film-forming resin is selected from one or more of polycaprolactone, caprolactone-lactic acid copolymer, poly (octylglycol citrate).
Preferably, the film-forming resin is polycaprolactone.
Further preferably, the polycaprolactone has an average molecular weight of 60000-80000.
In one embodiment, the titanium dioxide is selected from one of rutile titanium dioxide and anatase titanium dioxide.
Preferably, the titanium dioxide is anatase titanium dioxide. For example, the model is BA01-01 from the blue chemical industry of the gallery.
The applicant finds that the added titanium dioxide, in particular anatase titanium dioxide, has good shielding performance, good color rendering, more cleaning writing and more vivid color, and the band gap width of the anatase titanium dioxide is larger than that of rutile type, and photo-generated electrons and holes are not easy to be compounded on the surface, so that the anatase titanium dioxide has higher photocatalytic activity, can directly utilize ultraviolet light in sunlight to carry out photocatalytic degradation, and does not cause secondary pollution. However, the anatase titanium dioxide is not easy to disperse and writing is not smooth enough, and applicants creatively find that in the experimental process, the average molecular weight of film-forming resin, especially polycaprolactone, is controlled to be 60000-80000, the writing feeling is good, and the cleaning effect is good. The polycaprolactone has elasticity, can be erased in the form of a relatively large elastic film during erasure, and the part in the pit can be pulled up together by the external resin film without breaking, so that the part in the pit can be wiped clean as well, the polycaprolactone has biodegradability, and the resin film can be degraded after being erased if flowing into the environment, so that plastic pollution can not be caused to the environment. When the average molecular weight of polycaprolactone is 60000-80000, the number of chain segments contained in a molecular chain is large, in order to realize the migration of the center of gravity, the interfacial tension between solid and liquid can be reduced under the action of an emulsifying agent and a solvent, the dispersion of titanium dioxide is ensured by effectively wetting particles, when the average molecular weight of polycaprolactone is small, the migration resistance of the chain segments is small, the smoothness is good, but the film forming is slow, the writing is easy to touch the handwriting which is not dried yet, the plate surface is not clean, and when the average molecular weight of polycaprolactone is large, the migration resistance of the chain segments is large, the dispersion of the titanium dioxide is uneven, the writing is not smooth, and the ink breaking is easy.
In one embodiment, the aqueous pigment includes, but is not limited to, C.I. pigment black 7, C.I. pigment black 11, C.I. pigment black 1, C.I. pigment yellow 3, C.I. pigment yellow 12, C.I. pigment yellow 13, C.I. pigment yellow 14, C.I. pigment yellow 17, C.I. pigment yellow 35, C.I. pigment yellow 37, C.I. pigment yellow 42, C.I. pigment yellow 55, C.I. pigment yellow 95, C.I. pigment yellow 97, C.I. pigment yellow 98, C.I. pigment yellow 100, C.I. pigment yellow 110, C.I. pigment yellow 117, C.I. pigment yellow 120, C.I. pigment yellow 155, C.I. pigment red 1, C.I. pigment red 2, C.I. pigment red 3, C.I. pigment red 5, C.I. pigment red 7, C.I. pigment red 22, C.I. pigment red 23, C.I. pigment blue 31, C.I. pigment red 31, C.I. pigment blue 1, C.I. pigment blue 15, the addition can be performed by those skilled in the art according to actual requirements.
In one embodiment, the emulsifier is selected from one or more of polyvinyl alcohol, gelatin, span80, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, tween 80.
Preferably, the emulsifier is Tween80, CAS accession number: 9005-65-6.
In one embodiment, the dispersant is selected from one or more of AEO-8, AEO-9, AEO-10, AEO-15, DISPERBYK-110, DISPERBYK-142, DISPERBYK-160, DISPERBYK-161, polyethylene glycol 200, polyethylene wax.
Preferably, the dispersant is DISPERBYK-110, such as available from Jinan Santa and chemical industries, inc., model number DISPERBYK-110.
In one embodiment, the stabilizer is selected from one or more of sodium iminodisuccinate, sodium hydroxymethyl cellulose and sodium alginate.
Preferably, the stabilizer is a compound of sodium hydroxymethyl cellulose and sodium alginate, and the mass ratio is (5-10): 1.
in one embodiment, the leveling agent is selected from one or more of hydrophobic polyurethane, polyacrylic acid and carboxymethyl cellulose, BYK-333, BYK-307, BYK-377, BYK-378, BYK-352, BYK-354 and BYK-358.
Preferably, the leveling agent is carboxymethyl cellulose.
In one embodiment, the humectant is selected from any one of propylene glycol, glycerol, ethylene glycol.
In one embodiment, the solvent is selected from one or more of dichloromethane, acetone, ethyl acetate.
Preferably, the solvent is dichloromethane.
In one embodiment, the mass ratio of film-forming resin to solvent is (1-3): (7-9).
The invention also discloses a preparation method of the degradable liquid chalk, which comprises the following steps:
(1) Dissolving film-forming resin in a solvent to obtain a solution a; then adding the solution a into water containing an emulsifying agent and stirring at a high speed to obtain emulsion b; evaporating the solvent in the solution b by means of decompression or heating to obtain a residue as emulsion c;
(2) Adding titanium dioxide, a dispersing agent and pigment into water, and stirring or grinding and dispersing at high speed to obtain a dispersing liquid;
(3) Adding the dispersion liquid obtained in the step (2) and a stabilizer and a humectant into the emulsion c obtained in the step (1), and uniformly dispersing in a high-speed shearing dispersing machine at a high speed to obtain the liquid chalk.
The beneficial effects are that:
1. by adding the anatase titanium dioxide, the obtained liquid powder has good shielding performance, good color rendering, cleaner writing and more vivid color.
2. By adding polycaprolactone and controlling the average molecular weight to 60000-80000, the writing feeling is good, the cleaning effect is good, the writing is easy to erase, the uneven writing surface is also good in erasable effect, and the film forming substances falling off after erasing can be degraded in biology or other forms, so that plastic pollution can be avoided.
3. Under the action of the dispersing agent and the humectant, the pen point keeps moist, and the pen point can not be dried after being placed for a long time without being covered by the pen cap, so that smooth writing is not realized.
Detailed Description
Example 1
The embodiment 1 discloses a degradable liquid chalk, which is prepared from the following raw materials in parts by weight: 8 parts of polycaprolactone, 8 parts of titanium dioxide, 0.5 part of water-based pigment, 0.5 part of Tween80, 1 part of dispersing agent, 1 part of stabilizer, 0.5 part of flatting agent, 1 part of humectant, 33 parts of deionized water and 30 parts of dichloromethane.
The polycaprolactone is purchased from Shenzhen Guanghua Wenyu Co., ltd, model Esun600C and average molecular weight 60000.
The titanium dioxide is anatase titanium dioxide, and is purchased from the blue chemical industry of the gallery, and the model is BA01-01.
The aqueous pigment is C.I. pigment Red 7, CAS number 6471-51-8.
Tween80, CAS accession numbers: 9005-65-6.
The dispersant is DISPERBYK-110, available from Jinan Sheng and chemical industry Co., ltd, and the model is DISPERBYK-110.
The stabilizer is a compound of sodium hydroxymethyl cellulose and sodium alginate, and the mass ratio is 5:1.
the leveling agent is carboxymethyl cellulose, and is purchased from Shandong national chemical Co., ltd., CAS number 9000-11-7.
The humectant is propylene glycol.
The embodiment 1 on the other hand discloses a preparation method of the liquid chalk, which comprises the following steps:
step 1: firstly, 8 parts of polycaprolactone is taken to be dissolved to obtain a polycaprolactone solution, and the polycaprolactone solution is dissolved in 30 parts of dichloromethane to obtain a solution a. Then, the solution a was added to a beaker containing 0.5 parts of Tween80 and 23 parts of deionized water under high-speed stirring to obtain emulsion b, and then methylene chloride was removed by decompression to obtain emulsion c.
Step 2: 8 parts of titanium dioxide, 0.5 part of water-based pigment and 1 part of dispersing agent are added into 10 parts of deionized water under the condition of high-speed stirring to obtain a dispersion liquid.
Step 3: and (3) adding the dispersion liquid obtained in the step (2), 1 part of stabilizer, 1 part of flatting agent and 1 part of humectant into the emulsion a, and stirring and dispersing at a high speed to obtain the liquid chalk.
Example 2
The embodiment 2 discloses a degradable liquid chalk, which is prepared from the following raw materials in parts by weight: 20 parts of polycaprolactone, 30 parts of titanium dioxide, 3 parts of water-based pigment, 4 parts of Tween80, 3 parts of dispersing agent, 2 parts of stabilizer, 2 parts of leveling agent, 3 parts of humectant, 76 parts of deionized water and 50 parts of dichloromethane.
The polycaprolactone is purchased from Shenzhen Guanghua Wenyu Co., ltd, model Esun600C and average molecular weight 60000.
The titanium dioxide is anatase titanium dioxide, and is purchased from the blue chemical industry of the gallery, and the model is BA01-01.
The aqueous pigment is C.I. pigment Red 7, CAS number 6471-51-8.
Tween80, CAS accession numbers: 9005-65-6.
The dispersant is DISPERBYK-110, available from Jinan Sheng and chemical industry Co., ltd, and the model is DISPERBYK-110.
The stabilizer is a compound of sodium hydroxymethyl cellulose and sodium alginate, and the mass ratio is 10:1.
the leveling agent is carboxymethyl cellulose, and is purchased from Shandong national chemical Co., ltd., CAS number 9000-11-7.
The humectant is glycerol.
The embodiment 2 on the other hand discloses a preparation method of the liquid chalk, which comprises the following steps:
step 1: firstly, 20 parts of polycaprolactone is taken to be dissolved to obtain a polycaprolactone solution, and the polycaprolactone solution is dissolved in 50 parts of dichloromethane to obtain a solution a. Then, the solution a was added to a beaker containing 4 parts of Tween80 and 55 parts of deionized water under high-speed stirring to obtain emulsion b, and then methylene chloride was removed by decompression to obtain emulsion c.
Step 2: 30 parts of titanium dioxide and 3 parts of water-based pigment and 3 parts of dispersing agent are added into 21 parts of deionized water under high-speed stirring to disperse liquid.
Step 3: and (3) adding the dispersion liquid obtained in the step (2), 2 parts of stabilizer, 2 parts of flatting agent and 3 parts of humectant into the emulsion a, and stirring and dispersing at a high speed to obtain the liquid chalk.
Example 3
The embodiment 3 discloses a degradable liquid chalk, which comprises the following raw materials in parts by weight: 15 parts of polycaprolactone, 10 parts of titanium dioxide, 2 parts of water-based pigment, 2 parts of Tween80, 1 part of dispersing agent, 1 part of stabilizer, 1 part of flatting agent, 1 part of humectant, 67 parts of deionized water and 45 parts of dichloromethane.
The polycaprolactone is purchased from Shenzhen Guanghua Wenyu Co., ltd, model Esun600C and average molecular weight 60000.
The titanium dioxide is anatase titanium dioxide, and is purchased from the blue chemical industry of the gallery, and the model is BA01-01.
The aqueous pigment is C.I. pigment Red 7, CAS number 6471-51-8.
Tween80, CAS accession numbers: 9005-65-6.
The dispersant is DISPERBYK-110, available from Jinan Sheng and chemical industry Co., ltd, and the model is DISPERBYK-110.
The stabilizer is a compound of sodium hydroxymethyl cellulose and sodium alginate, and the mass ratio is 8:1.
the leveling agent is carboxymethyl cellulose, and is purchased from Shandong national chemical Co., ltd., CAS number 9000-11-7.
The humectant is propylene glycol.
The embodiment 3 on the other hand discloses a preparation method of the liquid chalk, which comprises the following steps:
step 1: firstly, 15 parts of polycaprolactone is taken to be dissolved to obtain a polycaprolactone solution, and the polycaprolactone solution is dissolved in 45 parts of dichloromethane to obtain a solution a. Then, the solution a was added to a beaker containing 2 parts of Tween80 and 45 parts of deionized water under high-speed stirring to obtain emulsion b, and then methylene chloride was removed by decompression to obtain emulsion c.
Step 2: 10 parts of titanium dioxide, 2 parts of water-based pigment and 1 part of dispersing agent are added into 22 parts of deionized water under high-speed stirring to disperse liquid.
Step 3: and (3) adding the dispersion liquid obtained in the step (2), 1 part of stabilizer, 1 part of flatting agent and 1 part of humectant into the emulsion a, and stirring and dispersing at a high speed to obtain the liquid chalk.
Example 4
The example 4 discloses a degradable liquid chalk, which comprises, by weight, 10 parts of polycaprolactone, 20 parts of titanium dioxide, 1.5 parts of Tween80, 1.5 parts of dispersing agent, 1.5 parts of stabilizer, 1 part of leveling agent, 1 part of humectant, 63.5 parts of deionized water and 40 parts of dichloromethane.
The polycaprolactone is purchased from Shenzhen Guanghua Wenyu Co., ltd, model Esun600C and average molecular weight 60000.
The titanium dioxide is anatase titanium dioxide, and is purchased from the blue chemical industry of the gallery, and the model is BA01-01.
Tween80, CAS accession numbers: 9005-65-6.
The dispersant is DISPERBYK-110, available from Jinan Sheng and chemical industry Co., ltd, and the model is DISPERBYK-110.
The stabilizer is a compound of sodium hydroxymethyl cellulose and sodium alginate, and the mass ratio is 8:1.
the leveling agent is carboxymethyl cellulose, and is purchased from Shandong national chemical Co., ltd., CAS number 9000-11-7.
The humectant is propylene glycol.
The embodiment 4 on the other hand discloses a preparation method of the liquid chalk, which comprises the following steps:
step 1: firstly, 10 parts of polycaprolactone is taken to be dissolved to obtain a polycaprolactone solution, and the polycaprolactone solution is dissolved in 40 parts of dichloromethane to obtain a solution a. Then, the solution a was added to a beaker containing 1.5 parts of Tween80 and 40 parts of deionized water under high-speed stirring to obtain emulsion b, and then methylene chloride was removed by decompression to obtain emulsion c.
Step 2: 20 parts of titanium dioxide and 1.5 parts of dispersing agent are added into 23.5 parts of deionized water under high-speed stirring to disperse liquid.
Step 3: and (3) adding the dispersion liquid obtained in the step (2), 1.5 parts of stabilizer, 1 part of flatting agent and 1 part of humectant into the emulsion a, and stirring and dispersing at a high speed to obtain the liquid chalk.
Example 5
This example 5 differs from example 3 in that the polycaprolactone is obtained from Shenzhen Guanghua West Inc., model Esun1000C, average molecular weight 100000.
Example 6
This example 6 differs from example 3 in that the polycaprolactone is obtained from Shenzhen Guanghua West Inc., model Esun500C, average molecular weight 50000.
Example 7
The difference between this example 7 and example 3 is that the titanium white powder is rutile titanium white powder, which is purchased from the Sichuan python and has the model R996.
Performance test:
1. writing test: the liquid chalks obtained in examples 1-7 were used to write on a whiteboard. The evaluation criteria were a: the handwriting is clear, the writing is smooth, the film forming is fast, and no scratch exists in the writing process; b: the handwriting is clearer, the writing is smoother, the film forming is quicker, and the handwriting is slightly scratched in the writing process; c: the handwriting is clear, the writing is not smooth, the film forming is slow, and the scratch is serious in the writing process.
2. Scrubbing test: and erasing the written notes. Evaluation criteria, a: the pen is very clean, can write immediately, and is clear and free from scratch; b: the pen is clean, has slight writing marks, can write immediately, is clear, and has slight scratch; c: not clean, not write on horses, or not clear.
| Writing test | Scrubbing test | |
| Example 1 | A | A |
| Example 2 | A | A |
| Example 3 | A | A |
| Example 4 | A | B |
| Example 5 | B | B |
| Example 6 | C | C |
| Example 7 | B | B |
Claims (8)
1. The degradable liquid chalk is characterized by comprising the following raw materials in parts by weight: 8-20 parts of film-forming resin, 8-30 parts of titanium dioxide, 0-3 parts of water-based pigment, 0.5-4 parts of emulsifier, 1-3 parts of dispersing agent, 1-2 parts of stabilizer, 0.5-2 parts of flatting agent, 1-3 parts of humectant, 33-76 parts of deionized water and 30-50 parts of solvent; the film-forming resin is polycaprolactone; the average molecular weight of the polycaprolactone is 60000-80000; the titanium dioxide is anatase titanium dioxide.
2. The liquid chalk of claim 1, wherein the emulsifier is selected from one or more of polyvinyl alcohol, gelatin, span80, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, tween 80.
3. The liquid chalk of claim 1, wherein the dispersant is selected from one or more of AEO-8, AEO-9, AEO-10, AEO-15, DISPERBYK-110, DISPERBYK-142, DISPERBYK-160, DISPERBYK-161, polyethylene glycol 200, polyethylene wax.
4. The liquid chalk of claim 1, wherein the stabilizer is selected from one or more of sodium iminodisuccinate, sodium hydroxymethyl cellulose and sodium alginate.
5. The liquid chalk of claim 1, wherein the leveling agent is selected from one or more of butyl cellulose, hydrophobic polyurethane, polyacrylic and carboxymethyl cellulose, BYK-333, BYK-307, BYK-377, BYK-378, BYK-352, BYK-354, and BYK-358.
6. The liquid chalk of claim 1, wherein the humectant is selected from one of propylene glycol, glycerol, and ethylene glycol.
7. The liquid chalk of claim 1, wherein the solvent is selected from one or more of methylene chloride, acetone, ethyl acetate.
8. A method of preparing a liquid chalk according to any of claims 1-7, comprising the steps of:
(1) Dissolving film-forming resin in a solvent to obtain a solution a; then adding the solution a into water containing an emulsifying agent and stirring at a high speed to obtain emulsion b; evaporating the solvent in the solution b by means of decompression or heating to obtain a residue as emulsion c;
(2) Adding titanium dioxide, a dispersing agent and pigment into water, and stirring or grinding and dispersing at high speed to obtain a dispersing liquid;
(3) And (3) adding the dispersion liquid obtained in the step (2), a stabilizer, a leveling agent and a humectant into the emulsion c obtained in the step (1), and uniformly dispersing in a high-speed shearing dispersing machine to obtain the liquid chalk.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827514A (en) * | 2011-06-17 | 2012-12-19 | 厦门市绿科达环保科技有限公司 | Erasable white ink for dustless pen and preparation method |
| CN110818938A (en) * | 2019-12-06 | 2020-02-21 | 东莞市超智新材料有限公司 | Preparation method of matte writing film containing particles and matte writing film |
| CN113004744A (en) * | 2021-03-18 | 2021-06-22 | 广州天禧科技有限公司 | Washable biomaterial ink |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827514A (en) * | 2011-06-17 | 2012-12-19 | 厦门市绿科达环保科技有限公司 | Erasable white ink for dustless pen and preparation method |
| CN110818938A (en) * | 2019-12-06 | 2020-02-21 | 东莞市超智新材料有限公司 | Preparation method of matte writing film containing particles and matte writing film |
| CN113004744A (en) * | 2021-03-18 | 2021-06-22 | 广州天禧科技有限公司 | Washable biomaterial ink |
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