CN105367808A - Preparation method of sodium alginate solution used for ink-jet printing ink - Google Patents
Preparation method of sodium alginate solution used for ink-jet printing ink Download PDFInfo
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- CN105367808A CN105367808A CN201510926172.6A CN201510926172A CN105367808A CN 105367808 A CN105367808 A CN 105367808A CN 201510926172 A CN201510926172 A CN 201510926172A CN 105367808 A CN105367808 A CN 105367808A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
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Abstract
The invention discloses a preparation method of a sodium alginate solution used for ink-jet printing ink. The preparation method comprises following steps: brown alga is immersed in water, and is washed; sodium carbonate is added into the processed brown alga for digestion reaction, and a glue solution is obtained via diluting with water; the glue solution is subjected to separation and purification so as to obtain a clear glue liquid; the clear glue liquid is subjected to acid coagulation reaction so as to obtain alginic acid; an organic solvent is used for dehydration, and then the organic solvent is removed; dehydrated alginic acid is smashed, is subjected to first heating so as to reduce viscosity, sodium hydroxide is added for neutralizing alginic acid, mass concentration is adjusted to be 5% with purified water, an obtained mixture is subjected to secondary heating so as to reduce viscosity, and is allowed to stand; after that a preservative is added, diatomite is used for filter pressing so as to obtain the finished product sodium alginate solution. The preparation method is simple; cost is low; and the obtained sodium alginate solution is transparent, and is low in viscosity, high in purity, and excellent in fluidity.
Description
Technical field
The invention belongs to ink-jet printing ink technical field, be specifically related to a kind of preparation method meeting the sodium alginate soln of viscosity needed for ink-jet printing ink and purity.
Background technology
Along with textiles popular cycle shortens gradually, the quality of production requires to improve constantly, ordering amount number reduces gradually, traditional printing in textiles mode can not meet the growth requirement of textile industry, and the appearance of " short run, personalization, rapid reaction " digit printing and development can meet the following rhythm produced fast.
Digital ink-jet printedly growing up on inkjet technology basis, is a kind of stamp mode becoming the principle of drop based on tiny fluid breaks.Ink-jet printed have the different of essence from Conventional decal: ink-jet printed is a kind of contactless stamp, and decalcomania is directly mixed to form at fabric face according to the microscopic ink droplets of different colours.Therefore, the shape of ink droplet and size have very important impact to ink-jet printed quality.
Digital ink-jet printed ink is generally made up of pigment, solvent, dye solubilization agent, water-holding agent, water-proofing agent, viscosity modifier, tackiness agent, defoamer, siccative etc.Ink, except the viscosity to pigment purity, insoluble solid grain diameter and ink, surface tension, specific conductivity, stability, pH value and whipability etc. have specific requirement, also requires that the pattern that ink spray printing to fabric is formed must have good water-fastness, the multinomial performance requirement such as colour fastness and fabric feeling.
At present, reactive dye ink is carried out ink-jet printed, usually needs to carry out pre-treatment to fabric used, fully can not anchor at phenomenon on fiber to prevent imbibition phenomenon and dyestuff.And need additionally to add viscosity modifier in ink and ink droplet can be sprayed and not easily broken.The viscosity modifier of extra interpolation common as polyvinyl alcohol, polyvinyl alcohol cold water is insoluble, and the aqueous solution, when storing, occurs that poison becomes sometimes.
Therefore, a kind of reactive dye ink sodium alginate can promote the use situation of current ink thickening material, both can prevent imbibition phenomenon, and dyestuff is fully anchored on fiber, simplifies pretreatment procedure, saves pulping process, saves sodium alginate consumption simultaneously; Viscosity needed for ink can be provided again, can not shower nozzle be blocked and make textile printing clear patterns, stamp good hand touch.
Summary of the invention
The invention provides a kind of preparation method of ink-jet printing ink sodium alginate soln, be applied in ink-jet printing ink, easy to use, to shower nozzle without blocking, corrosion-free, good with dyestuff, auxiliary agent consistency, there is good storage stability, and Environmental Safety.
For achieving the above object, the present invention adopts following technical proposals to be achieved: a kind of preparation method of ink-jet printing ink sodium alginate soln, is to use brown alga to soak, wash; In brown alga, add sodium carbonate carry out digestion reaction, thin up obtains glue; Clear glue solution is obtained to glue separation, purifying; Acid cure reaction is carried out to clear glue solution, obtains Lalgine, adopt dehydration of organic solvent, then remove organic solvent; Lalgine after dehydration is pulverized, a heating, viscosity reducing degree, in hydro-oxidation sodium and Lalgine, add pure water and be adjusted to 5% mass concentration solution, second-heating viscosity reduction degree, after leaving standstill, add sanitas, use diatomite press filtration, obtain the finished product sodium alginate soln.
Further, the mass concentration of described the finished product sodium alginate soln is 3-6%, and soltion viscosity is 40-60mpa.s, and pH value is 6.8-8.0, and transparency is 80.0-100.0cm.
Further, the M/G ratio of described brown alga is 2.0-3.0, and the time of soaking is 4-6h.
Further, described digestion reaction temperature is 50-55 DEG C, the reaction times is 2-3h, and the mass ratio of brown alga and sodium carbonate is 10:2-3, is diluted with water to 100-130 times that viscosity Engler is 80-100s, dilution is dry brown alga quality.
Further, glue obtains clear glue solution after dissolved air flotation or centrifugation, and clear glue solution uses diatomite filtration, and diatomite granularity is 200-300 order, and diatomite quality is the 1-5 ‰ of clear glue solution quality.
Further, described acid cure reaction conditions is the mass concentration of hydrochloric acid is 10%-15%, and the mass ratio of hydrochloric acid and clear glue solution is 0.5-1.5:90-110, and the acid cure time is 20-30min.
Further, the organic solvent that dehydration adopts is ethanol concn is 20-40 ° of alcohol mother liquor, and after dehydration, Lalgine water content is 50-60%; Then vacuum removes organic solvent, and temperature is 50-60 DEG C, and the time is 20-40min.
Further, in a heating, viscosity reducing degree step, Heating temperature is 60-70 DEG C, intermittent stirring 2-6h.
Further, in second-heating viscosity reduction degree step, Heating temperature is 50-70 DEG C, intermittent stirring 6-10h.
Further, press filtration diatomite granularity is 1000-1500 order, and diatomite quality is the 1-3 ‰ of adhesive liquid quantity.
Advantage of the present invention and positively effect are: in the preparation of sodium alginate soln of the present invention, and brown alga is selected rational M/G ratio and uses hydrochloric acid acid cure legal system standby, guarantees that product has excellent mobility.The advantage utilizing detailed catalogue number high-quality diatomite self to have many natural micropores carries out separation and purification to glue, then uses hydrochloric acid to carry out acid cure reaction to the clear glue solution after filtration, can remove the impurity such as carbohydrate gum; Use alcohol repeatedly to wash acid cure product and can remove inorganic salt, at utmost improve product purity, guarantee to block shower nozzle.By in and Working Procedure Controlling product pH value, guarantee the quality stability that product is good.Utilize the mode of heating to reduce Lalgine viscosity, guarantee to reach the viscosity needed for ink and purity; Utilize heating under vacuum remove alcohol, add sanitas and do not use the modes such as hydrogen peroxide to reduce viscosity, guarantee product good package stability.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail.
The preparation method of a kind of ink-jet printing ink sodium alginate soln of the present invention is:
1) choose brown alga and soak 4-6h, washing, the M/G ratio of described brown alga is 2.0-3.0; Select rational M/G ratio can guarantee that the finished product have excellent mobility;
2) in brown alga, add sodium carbonate and carry out digestion reaction, digestion reaction temperature is 50-55 DEG C, reaction times 2-3h, and the mass ratio of brown alga and sodium carbonate is 10:2-3; Digestion reaction product thin up is obtained glue, and the viscosity Engler of glue is 80-100s, is diluted to the 100-130 of dry brown alga quality doubly;
3) carry out separation and purification to glue, specifically adopt dissolved air flotation or centrifugation to obtain clear glue solution to glue, use diatomite filtration to clear glue solution, described diatomite granularity is 200-300 order, and diatomite quality is the 1-5 ‰ of clear glue solution quality;
4) clear glue solution after filtering uses hydrochloric acid to carry out acid cure reaction, and obtain Lalgine, the mass concentration of hydrochloric acid is 10%-15%, and the mass ratio of hydrochloric acid and clear glue solution is 0.5-1.5:90-110, and the acid cure time is 20-30min;
5) with an organic solvent help dehydration, described organic solvent is ethanol concn is 20-40 ° of alcohol mother liquor, and after dehydration, Lalgine water content is 50-60%; Then vacuum removes organic solvent, and temperature is 50-60 DEG C, and the time is 20-40min;
6) Lalgine after dehydration is pulverized, be crushed to by bulk cotton-shaped.A heating, viscosity reducing degree, Heating temperature is 60-70 DEG C, intermittent stirring 2-6h, stirs 20min every 1 hour.
7) in hydro-oxidation sodium and Lalgine be 6.8-8.0 to pH value, obtain sodium alginate, adding the mass concentration that pure water is adjusted to sodium alginate soln is 3-6%; Second-heating viscosity reduction degree, Heating temperature is 50-70 DEG C, and 6-10h is stirred at interval, stir 20min every 1 hour, after leaving standstill, add sanitas, use diatomite press filtration, obtain the finished product, described diatomite granularity is 1000-1500 order, and diatomite quality is the 1-3 ‰ of sodium alginate adhesive liquid quantity.
The mass concentration of the sodium alginate that the present invention prepares is 3-6%, and soltion viscosity is 40-60mpa.s, and pH value is 6.8-8.0, and transparency is 80.0-100.0cm.
Described sanitas is sterilizing solution CI (effective constituent is isothiazolinone derivatives), and sanitas consumption is the 2.5-3.5 ‰ of sodium alginate quality.
The outstanding advantage that sodium alginate soln of the present invention is used in ink has 3 points: first is that preparation technology is simple, cost is low, and product can prevent imbibition phenomenon after adding, dyestuff is fully anchored on fiber, simplify pretreatment procedure, save pulping process, reduce sodium alginate usage quantity simultaneously, save human and material resources, reduce a part of client's use cost; Second point is that its viscosity meets required viscosity in ink, and purity is high, can not block, corrode shower nozzle, and its rheological is good, good with fastness, armful water-based is good; Be thirdly easy to use, excellent storage stability, meets environmental requirement, and after application, printed mark sharpness is good, dye yield is high, good hand touch.
Embodiment 1
Get 100g kelp soaking 4h, the M/G ratio of brown alga is 2.0, the after washing 3 times of cutting the dish.Digestion reaction: add sodium carbonate, the mass ratio of brown alga and sodium carbonate is 10:2, temperature of reaction 50 DEG C, reaction times 3h, and the viscosity Engler being diluted to glue is 90s, centrifuge, diatomite filtration, and diatomaceous granularity is 200 orders, and diatomite consumption is 3 ‰.Acid cure is reacted: by glue: hydrochloric acid (mass concentration 10%) quality is 100:0.5 acid cure, leaves standstill 20min, obtains Lalgine.Lalgine is used 20 ° of alcohol mother liquor by dewaterings, after dehydration, Lalgine moisture is 52%.After being pulverized by Lalgine after dehydration, 50 DEG C of vacuum remove alcohol, are heated to 60 DEG C, stir 4h, stir 20min every 1 hour.Add sodium hydroxide and be adjusted to product pH=7.7, obtain sodium alginate.Measure solid content, adding the mass concentration that pure water is adjusted to sodium alginate soln is 5%, is heated to 55 DEG C, stirs 8h, stirred 20min every 1 hour, to required viscosity.Leave standstill, add 2.5 ‰ sanitass (relative to sodium alginate quality), diatomite press filtration, diatomaceous granularity is 1000 orders, and diatomite quality is 1.5 ‰ of sodium alginate adhesive liquid quantity, obtains the finished product.
The finished product sodium alginate soln viscosity 45mpa.s, pH value 7.7, transparency 92cm, calcium contents is 0.
Embodiment 2
Get 100g kelp soaking 5h, the M/G ratio of brown alga is 2.0; To cut the dish after washing 3 times.Digestion reaction: add sodium carbonate, the mass ratio of brown alga and sodium carbonate is 10:2.5, temperature of reaction 52 DEG C, reaction times 2.5h, the viscosity Engler being diluted to glue is 95s, centrifuge, diatomite filtration, diatomaceous granularity is 300 orders, and diatomite consumption is 1 ‰.Acid cure is reacted: by glue: hydrochloric acid (mass concentration 10%)=95:1 acid cure, leaves standstill 25min, obtains Lalgine.Lalgine is used 30 ° of alcohol mother liquor by dewaterings, after dehydration, Lalgine moisture is 55%.After being pulverized by Lalgine after dehydration, 55 DEG C of vacuum dispel alcohol, are heated to 65 DEG C, stir 5h, stir 20min every 1 hour.Add sodium hydroxide and be adjusted to product pH=7.6.Measure solid content, add pure water and be adjusted to 6% mass concentration solution, be heated to 60 DEG C, stir 9h, stirred 20min every 1 hour, to required viscosity.Leave standstill, add 3 ‰ sanitass (relative to sodium alginate quality), diatomite press filtration, described diatomite granularity is 1200 orders, and diatomite quality is 1 ‰ of sodium alginate adhesive liquid quantity, obtains the finished product.
The finished product sodium alginate soln viscosity 46mpa.s, pH value 7.6, transparency 92cm, calcium contents is 0.
Embodiment 3
Get 100g kelp soaking 6h, the M/G ratio of brown alga is 3.0; To cut the dish after washing 3 times.Digestion reaction: add sodium carbonate, the mass ratio of brown alga and sodium carbonate is 10:3, temperature of reaction 55 DEG C, reaction times 2h, and the viscosity Engler being diluted to glue is 80s, centrifuge, diatomite filtration, and diatomaceous granularity is 300 orders, and diatomite consumption is 5 ‰.Acid cure is reacted: by glue: hydrochloric acid (mass concentration 10%)=110:1.5 acid cure, leaves standstill 30min, obtains Lalgine.Lalgine is used 40 ° of alcohol mother liquor by dewaterings, after dehydration, Lalgine moisture is 60%.After being pulverized by Lalgine after dehydration, 60 DEG C of vacuum dispel alcohol, are heated to 68 DEG C, stir 6h, stir 20min every 1 hour.Add sodium hydroxide and be adjusted to product pH=7.6.Measure solid content, add pure water and be adjusted to 3% mass concentration solution, be heated to 70 DEG C, stir 8h, stirred 20min every 1 hour, to required viscosity.Leave standstill, add 3.5 ‰ sanitass (relative to sodium alginate quality), diatomite press filtration, described diatomite granularity is 1500 orders, and diatomite quality is 2 ‰ of sodium alginate adhesive liquid quantity, obtains the finished product.
The finished product sodium alginate soln viscosity 46mpa.s, pH value 7.6, transparency 92cm, calcium contents is 0.
Obtained liquid thickener is stored 1 month under 30 DEG C of conditions, and viscosity (46mpa.s), pH (7.6), transparency (92cm) all do not change, and have good storage stability.
Above embodiment is only several in the several preferred implementation of the present invention, it should be pointed out that and the invention is not restricted to above-described embodiment; For the person of ordinary skill of the art, still the technical scheme described in previous embodiment can be modified, or equivalent replacement is carried out to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of the present invention's technical scheme required for protection.
Claims (10)
1. a preparation method for ink-jet printing ink sodium alginate soln, is characterized in that, uses brown alga to soak, wash; In brown alga, add sodium carbonate carry out digestion reaction, thin up obtains glue; Clear glue solution is obtained to glue separation, purifying; Acid cure reaction is carried out to clear glue solution, obtains Lalgine, adopt dehydration of organic solvent, then remove organic solvent; Lalgine after dehydration is pulverized, a heating, viscosity reducing degree, in hydro-oxidation sodium and Lalgine, add pure water and be adjusted to 5% mass concentration solution, second-heating viscosity reduction degree, after leaving standstill, add sanitas, use diatomite press filtration, obtain the finished product sodium alginate soln.
2. a kind of ink-jet printing ink sodium alginate soln according to claim 1, it is characterized in that: the mass concentration of described the finished product sodium alginate soln is 3-6%, soltion viscosity is 40-60mpa.s, and pH value is 6.8-8.0, and transparency is 80.0-100.0cm.
3. a kind of ink-jet printing ink sodium alginate soln according to claim 1, is characterized in that: the M/G ratio of described brown alga is 2.0-3.0, and the time of soaking is 4-6h.
4. a kind of ink-jet printing ink sodium alginate soln according to claim 1, it is characterized in that: described digestion reaction temperature is 50-55 DEG C, the reaction times is 2-3h, the mass ratio of brown alga and sodium carbonate is 10:2-3, is diluted with water to 100-130 times that viscosity Engler is 80-100s, dilution is dry brown alga quality.
5. a kind of ink-jet printing ink sodium alginate soln according to claim 1, it is characterized in that: glue obtains clear glue solution after dissolved air flotation or centrifugation, clear glue solution uses diatomite filtration, and diatomite granularity is 200-300 order, and diatomite quality is the 1-5 ‰ of clear glue solution quality.
6. a kind of ink-jet printing ink sodium alginate soln according to claim 1, it is characterized in that: described acid cure reaction conditions is the mass concentration of hydrochloric acid is 10%-15%, the mass ratio of hydrochloric acid and clear glue solution is 0.5-1.5:90-110, and the acid cure time is 20-30min.
7. a kind of ink-jet printing ink sodium alginate soln according to claim 1, is characterized in that: the organic solvent that dehydration adopts is ethanol concn is 20-40 ° of alcohol mother liquor, and after dehydration, Lalgine water content is 50-60%; Then vacuum removes organic solvent, and temperature is 50-60 DEG C, and the time is 20-40min.
8. a kind of ink-jet printing ink sodium alginate soln according to claim 1, is characterized in that: in a heating, viscosity reducing degree step, Heating temperature is 60-70 DEG C, intermittent stirring 2-6h.
9. a kind of ink-jet printing ink sodium alginate soln according to claim 1, is characterized in that: in second-heating viscosity reduction degree step, Heating temperature is 50-70 DEG C, intermittent stirring 6-10h.
10. a kind of ink-jet printing ink sodium alginate soln according to claim 1, is characterized in that: press filtration diatomite granularity is 1000-1500 order, diatomite quality is the 1-3 ‰ of adhesive liquid quantity.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105803827A (en) * | 2016-04-01 | 2016-07-27 | 华南师范大学 | Ink-jet ink and application thereof |
| CN108193526A (en) * | 2017-12-26 | 2018-06-22 | 青岛明月海藻集团有限公司 | A kind of digital printing gum of activity and preparation method thereof |
| CN109797577A (en) * | 2019-01-10 | 2019-05-24 | 江苏明月海洋生物科技有限公司 | A kind of sodium alga acid printing paste preparation method of pure cotton knitting cloth |
| CN111925688A (en) * | 2020-07-09 | 2020-11-13 | 青岛明月海藻集团有限公司 | Paste for ceramic screen printing and preparation method thereof |
-
2015
- 2015-12-11 CN CN201510926172.6A patent/CN105367808A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 吴疆，童应凯，杨红澎: "《生物分离实验技术》", 30 September 2009 * |
| 李群，赵昔慧: "《天然产物在绿色纺织品生产中的应用》", 30 March 2008 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105803827A (en) * | 2016-04-01 | 2016-07-27 | 华南师范大学 | Ink-jet ink and application thereof |
| CN108193526A (en) * | 2017-12-26 | 2018-06-22 | 青岛明月海藻集团有限公司 | A kind of digital printing gum of activity and preparation method thereof |
| CN109797577A (en) * | 2019-01-10 | 2019-05-24 | 江苏明月海洋生物科技有限公司 | A kind of sodium alga acid printing paste preparation method of pure cotton knitting cloth |
| CN111925688A (en) * | 2020-07-09 | 2020-11-13 | 青岛明月海藻集团有限公司 | Paste for ceramic screen printing and preparation method thereof |
| CN111925688B (en) * | 2020-07-09 | 2022-08-16 | 青岛明月海藻集团有限公司 | Paste for ceramic screen printing and preparation method thereof |
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Application publication date: 20160302 |