WO2023083238A1 - 用于制备彩色洗衣粉的染料分散体及彩色洗衣粉的制备方法 - Google Patents

用于制备彩色洗衣粉的染料分散体及彩色洗衣粉的制备方法 Download PDF

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WO2023083238A1
WO2023083238A1 PCT/CN2022/131024 CN2022131024W WO2023083238A1 WO 2023083238 A1 WO2023083238 A1 WO 2023083238A1 CN 2022131024 W CN2022131024 W CN 2022131024W WO 2023083238 A1 WO2023083238 A1 WO 2023083238A1
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dye dispersion
washing powder
dye
dispersion
water
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PCT/CN2022/131024
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English (en)
French (fr)
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胡灏
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美利肯企业管理(上海)有限公司
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Publication of WO2023083238A1 publication Critical patent/WO2023083238A1/zh

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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
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
    • C09B67/0084—Dispersions of dyes
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/40—Dyes ; Pigments
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/50—Solvents

Definitions

  • the invention relates to the field of washing powder preparation, in particular to a dye dispersion for preparing colored washing powder and a method for preparing colored washing powder using the dye dispersion.
  • Laundry powder is an important detergent in daily life. With the diversification of consumer demand, colored laundry detergent emerged as the times require.
  • the usual washing powder production process is to mix detergent raw materials used for fabric cleaning purposes, such as various surfactants and detergent auxiliaries, to prepare a slurry, and then spray it through a high tower and dry it with hot air to obtain a product with a certain density and particle size.
  • Laundry powder granules In order to endow laundry detergent with more functions to meet diverse needs, various additives, such as enzymes, polymers, fragrances, non-ionic surfactants, etc., can also be mixed in the post-mixing stage to enrich product performance.
  • the existing preparation process in the field of colored washing powder involved in the present invention is usually a pre-mixing process, that is, the preparation and mixing of pigment raw materials and slurry before the powder spraying process.
  • the basic flow of the process is to add appropriate The proportion of a certain pigment raw material, after mixing evenly, spraying powder granulation to obtain uniform color washing powder granules.
  • Such a production process will cause the powder spraying tower to be polluted by pigments, which will affect the subsequent production of washing powder. Cleaning the powder spraying tower is also time-consuming and labor-intensive.
  • CN110846140A discloses a preparation process for colored washing powder. This process uses nonionic surfactants to disperse dyes. In the post-mixing process, atomize and spray on the surface of detergent powder particles. In this process, the content of non-ionic surfactant in the dye-non-ionic surfactant solution is required to be 90-99.5%. Such a high content range will affect the formula of detergent powder. The total content of surfactants in the middle, especially when facing the situation that non-ionic surfactants are not required to be added in the laundry powder-based powder formula, the application of this preparation method will be severely limited.
  • the after-mixing process still has quite obvious advantages in the preparation of colored laundry detergent.
  • the after-mixing process does not need to make large-scale improvements to the existing washing powder production line, and only needs to increase the spraying process to convert the prepared The color dispersion is sprayed on the washing powder base powder; on the other hand, the finishing process gives the washing powder additional color levels to meet individual needs.
  • the application of the after-mixing process is still limited at present, because it inevitably introduces the colorant dispersion into the original washing particles.
  • the introduction of the dye dispersion changes the composition of the washing powder as a whole. Therefore, when developing the pre-mixing process, the selection of the colorant dispersion is very important, and the selection of the colorant dispersion also directly affects the design of the color washing powder preparation method.
  • the invention provides a dye dispersion, which contains polyhydric alcohol and water-soluble dye dispersed therein.
  • the composition of the powder which means: the introduced pigment dispersion should contain as much pigment components as possible under a certain weight, and at the same time, it should be able to adapt to the material requirements of the post-mixing process, especially the viscosity requirements in the spraying process .
  • the inventor has noticed that the spraying process in the after-mixing process is inevitable.
  • the spraying device is often used to prepare white washing powder base powder and colored washing powder at the same time.
  • the colorless solution is switched to use, which requires that the colorant solution is not easy to cause staining of the equipment and is easy to clean.
  • the advantage of the after-mixing process is that it can prepare colored washing powder by additionally spraying coloring material dyeing, so it has the advantage that it is suitable for all current commercial washing powder base powder varieties as far as possible, and is compatible with various washing powders.
  • the type of surfactant is compatible with the variety of laundry detergent as the active ingredient of the detergency, so a combination of factors is required.
  • the inventor has also noticed that the introduction of water in the after-mixing process needs to add an additional drying process in the process, which is unfavorable for industrial production, so it is beneficial to develop dye dispersions and color washing powder preparation methods that do not contain water of.
  • the inventors selected a water-soluble dye system using polyalcohol as a dispersant as a dye dispersion to overcome the above-mentioned known problems.
  • the dye dispersion involved in the present invention has lower equipment contamination, is not easy to dye equipment, and is easy to clean; as a dispersant, polyhydric alcohol has a lower price than surfactants , can effectively improve the flexibility of the dye dispersion formulation; in addition, compared with surfactants, especially non-ionic surfactants, polyols have lower viscosity, which is also beneficial for the spraying process.
  • the dye dispersion involved in the present invention does not contain water, no additional drying process is required, which broadens the application scenarios of the present invention.
  • the inventors unexpectedly found that the viscosity of the dye dispersion using polymer pigments decreases with the concentration of the colorant in the dispersion, which makes the polymer pigments satisfy the formula because they do not need to be dispersed by surfactants.
  • the concentration of the colorant in the dispersion which makes the polymer pigments satisfy the formula because they do not need to be dispersed by surfactants.
  • the higher the concentration, the lower the viscosity it is possible to have a low concentration and a high colorant concentration. Therefore, the polymer pigment dispersion is the best choice for the preparation of color washing powder in the after-mixing process. The prospects are quite bright.
  • the present invention also provides a method for preparing colored washing powder, which comprises the steps of: preparing a dye dispersion and uniformly spraying the dye dispersion on the washing powder base powder, and the dye dispersion contains polyhydric alcohol and dispersed therein water-soluble dyes.
  • the inventors have found that the formulation of the dye dispersion used in the spraying process is highly compatible and has no risk of contaminating equipment.
  • the process of this method can be independent of the preparation process of conventional laundry powder set individually. This greatly broadens the application scenarios of post-processing technology.
  • the inventors have found that, if the dispersion does not contain additional water, it is advantageous for industrial production not to introduce an additional drying process to remove water after the spraying process.
  • polymer pigment dispersions especially polymer pigment-propylene glycol dispersions, can achieve better performance under industrially acceptable conditions.
  • the present invention also provides the use of a dye dispersion for preparing colored laundry powder and the colored laundry powder prepared by the method for preparing colored laundry powder in the present invention.
  • the dye dispersion of the present invention is a homogeneous substance formed by dispersing a water-soluble dye in a dispersion medium.
  • the water-soluble dyes of the present invention are a subset of pigments/colorants, including all macromolecular or small molecular coloring substances that can be dissolved in water.
  • the water-soluble dyes in the present invention are preferably polymer pigments.
  • a polymeric pigment is generally a colorant having at least one chromophore moiety attached to at least one oligomeric or polymeric chain, wherein said chain has at least three repeating units.
  • the oligomeric or polymeric constituents may be bound to the chromophore by any suitable means, such as by covalent bonds, ionic bonds or suitable electrostatic interactions.
  • polymeric pigments can be characterized as having an absorbance in the range of about 300 nm and about 900 nm, as measured by ultraviolet-visible spectroscopy.
  • the molecular weight of polymeric pigments is usually expressed as a molecular weight distribution. Accordingly, the molecular weight of polymeric pigments is usually reported as an average molecular weight determined by its molecular weight distribution.
  • the chromophoric group of a colorant can vary widely, and can include compounds characterized in the art as dyes or pigments. The actual groups used will depend largely on, for example, the desired color and color fastness characteristics.
  • the chromophoric group may be linked to at least one polyalkyleneoxy substituent via a suitable nitrogen, oxygen, sulfur, etc. linking moiety.
  • chromophores examples include nitroso, nitro, azo (including monoazo, disazo, trisazo, tetrasazo, polyazo, formazan, azomethine and their metal complexes ), 1,2-stilbene, diarylmethane, triarylmethane, xanthene acridine, quinoline, methine (including polymethine), thiazole, indamine, indophenol, azine, Thiazines, oxazines, aminoketones, hydroxyketones, anthraquinones (including anthrazoline, anthrone, anthrapyridone, anthrapyrimidine, flavanthrone, pyranthrone, benzoanthrone, perylene, perylene (perinone, naphthalimide and other structures formally related to anthraquinone), indigos (including thioindigo), phthalocyanine chromophores and mixtures thereof.
  • polyalkyleneoxy chains examples include polyalkyleneoxy chains.
  • polyalkyleneoxy generally refers to molecular structures containing the following repeating units: -CH 2 CH 2 O-, CH 2 CH 2 CH 2 O-, -CH 2 CH 2 CH 2 CH 2O- , -CH2CH ( CH3 ) O- , -CH2CH ( CH2CH3 )O- CH2CH2CH ( CH3 )O-, and any combination thereof.
  • Typical of such groups that can be attached to a chromophore are polyepoxides such as polyalkylene oxides and copolymers thereof.
  • Typical polyalkylene oxides and copolymers thereof useful in providing colorants include those made from alkylene oxide (alkylene oxide) monomers containing 2 to 20 carbon atoms, or more preferably 2 to 6 carbon atoms .
  • Examples include: polyethylene oxide; polypropylene oxide; polybutylene oxide; oxetanes; tetrahydrofuran; copolymers of polyethylene oxide, polypropylene oxide, and polybutylene oxide and other copolymers comprising block copolymers wherein the majority of the polymeric substituents are polyethylene oxide, polypropylene oxide and/or polybutylene oxide. Additionally, the average molecular weight of such polyalkyleneoxy groups can range from about 132 to about 10,000, preferably from 176 to about 5,000.
  • the precise chemical identity of the terminal groups on the polyalkyleneoxy groups may not be critical as long as the correct function of the colorant is composition dependent since the colorant generally may not be chemically bound to the carrier.
  • some of the most preferred colorants will be identified wherein certain end groups are identified. Such statements regarding terminal groups are not to be construed in any way as limiting the invention to its broader embodiments. According to such a most preferred embodiment, the colorant may be characterized as follows:
  • R is an organic chromophoric group
  • A is a linking part in the organic chromophoric group and is selected from N, O, S or CO 2
  • the alkylene moiety of the alkyleneoxy component contains about 2 to about 4 carbon atoms
  • n is an integer from 2 to about 230
  • m is 1 when A is O, S, CO
  • m is 1 or 2 when A is N
  • x is an integer from 1 to 5
  • n The product of multiplying x times m(nmx) is 2 to about 230
  • R is a member selected from:
  • R is H, an alkyl group containing up to about 20 carbon atoms, or a carboxy-terminated alkyl group containing up to about 20 carbon atoms
  • j and k is OH, OM, or OR 3
  • M is the cationic moiety of an alkali metal, alkaline earth metal, transition metal (eg, nickel, etc.), or ammonium
  • R 3 is an alkyl group containing up to about 20 carbon atoms.
  • the oligomeric component may be any suitable component, including, but not limited to, an oligomeric component selected from (i) comprising a minimum of three selected from the group consisting of C2 - C20 alkyleneoxy groups, glycidol groups and oligomers of monomeric or repeating units of glycidyl groups, (ii) aromatic or aliphatic oligoesters according to structure (I):
  • R 2 and R 3 are independently selected from hydrogen and C 1 -C 10 alkyl, f is an integer between 1 and 10 inclusive, and g is between 1 and 20 Any positive integer or fraction between and including 1 and 20.
  • suitable values for g include both integers and fractions, since the length of the oligomeric components on a single polymeric pigment molecule can vary. Thus, for a given sample or collection of polymer pigment molecules, the value of g represents the average length of the ester chain.
  • the polymeric pigment may comprise one or more oligomeric components composed of three or more oxirane monomer groups.
  • Exemplary polymeric pigments include polymer pigments and Polymer pigments, of which polymer pigments is more preferable.
  • Polymer pigments are characterized in that they are water-soluble, non-staining colorants. They are widely used in laundry detergents, fabric softeners, and other consumer and industrial cleaning products. Polymeric pigments are typically clear liquid colorants that exhibit excellent solubility in water, are compatible with other chemicals present in their end-use formulations, and are easy to handle. Polymeric pigments can be used to provide color in both aqueous and solid systems. The unique polymeric properties of polymer pigments provide lower staining of skin, textiles, hard surfaces, equipment and more.
  • Polymer pigments are liquid colorants developed especially for washable applications, such as in markers, paints and other art products. They contain no heavy metals, are non-toxic, and have excellent non-staining properties on skin, fabrics, and other surfaces. Polymeric pigments have excellent compatibility with water-based ink formulations and provide vibrant colors.
  • Dyes within the scope of the present invention can also be selected from one or more of the following classes of colorants can be suitable for use as colorants in color particles: acid dyes, basic dyes, direct dyes, solvent dyes, vat dyes, Mordant dyes, indigo dyes, reactive dyes, disperse dyes, sulfur dyes, fluorescent dyes, natural colorants, etc.
  • the weight percentage of the water-soluble dye in the dye dispersion is 0-95%, and the above weight percentage is based on the total weight of the dye dispersion. In some preferred embodiments, the weight percentage of the water-soluble dye in the dispersion is 5-40%, more preferably 10-20%. This content range endows the dye dispersion with a wide color range, which makes the color laundry powder prepared from the dye dispersion have a wider selection range in color concentration, and at the same time takes into account the balance of the viscosity of the dye dispersion, which is suitable for post-mixing process in the spraying process.
  • polyols are selected as dispersants to disperse water-soluble dyes.
  • polyhydric alcohols include propylene glycol and glycerin.
  • the amount of polyol added or its percentage in the dye dispersion is determined according to the selected water-soluble dye. When choosing a water-soluble dye with a wider solubility range, the content range of the dispersant can be larger.
  • the inventors have found that controlling the viscosity of the above-mentioned dye dispersion is important for the spraying process and even the entire color washing powder production after-mixing process. Considering various factors such as dyeing performance and dispersion concentration, the inventors have found that the viscosity range does not exceed 80mPa.s It is preferred, taking into account the concentration of the colorant in the dye dispersion, the requirements of the spraying process, and the influence of temperature on the viscosity, etc., preferably no more than 60mPa.s, especially preferably 10 to 60mPa.s; for polymer pigment dispersions, A further preferred viscosity range is 20-40 mPa.s.
  • the dye dispersion does not contain surfactants or water.
  • the reason for the above-mentioned exclusive limitation is that the inventors have found that polyols have good dispersion performance for water-soluble dyes. In this case, there is no need to add surfactants or water to improve the dispersion of the dispersion system, and to give the dye dispersion more Good formulation flexibility.
  • the dye dispersion is a polymer pigment-propylene glycol dispersion with a viscosity of 10-60 mPa.s, wherein the weight percentage of the polymer pigment is 0.01-40%.
  • the method for preparing colored washing powder in the present invention comprises preparing the dye dispersion as described above, and uniformly spraying the dye dispersion on the washing powder base powder.
  • the washing powder base powder, its preparation method, and the operation steps and processes involved in the preparation of the dye dispersion in the present invention are known in the art.
  • the method of evenly spraying the dye dispersion on the base powder covers the method of using industrial nozzles, atomizers and other dispersion equipment to coat the liquid dispersion on the outside of the laundry powder base powder.
  • the method for preparing colored washing powder in the present invention has been developed.
  • the dye dispersion used does not contain water or surfactants, no additional drying process is required after the dye dispersion is uniformly sprayed on the laundry powder base powder to remove Moisture simplifies the process and effectively reduces the cost of industrial production.
  • the dye dispersion used is a polymer pigment-propylene glycol dispersion with a viscosity of 10-60 mPa.s, wherein the weight percentage of the polymer pigment is 0.01-40%.
  • Table 1 The dye dispersion preparation composition of embodiment and comparative example
  • A1, A3, A5, A7, A9 and A11 are all dye dispersions with propylene glycol as the dispersion medium.
  • water-soluble dyes such as FBL, Acid Red 52, and Tartrazine have poor dispersibility at concentrations of 20% or 40%, and the mixture of water-soluble dyes presents a paste during the preparation process.
  • concentration of permanent dyes is adjusted accordingly to 2% or 4%; but at 20% or even 40% by weight, Polymer pigment dispersion performed well.
  • B1, B3, B5, B7, B9 and B11 are all dye dispersions using AOE9 (a commercially available nonionic surfactant) as the dispersion medium.
  • AOE9 a commercially available nonionic surfactant
  • Water-soluble dyes such as Fast Green Blue (FBL), Acid Red 52, and Tartrazine cannot be uniformly dispersed at a concentration of 2% or 4% to form a uniform substance, showing unacceptable dispersion performance; but at 20% and 4% 40% by weight, the Polymer pigment dispersibility is good.
  • the viscosity of the dispersion decreased with the increase of the polymer pigment concentration.
  • the dispersion viscosity drops to about 20mPa.s.
  • the viscosity of the polymer pigment dispersion ranges from 10 to 60 mPa.s at a concentration of 0.01% to 40%.
  • Polymer pigments can help color laundry detergents improve color performance while reducing the viscosity of spray colorant dispersions. This is beneficial for improving the quality of colored washing powder and reducing industrial production costs.
  • Visible, A6 and A10 correspond to Polymer pigment dye dispersions have lower equipment contamination and equipment damage.
  • water-soluble dyes such as FBL, Acid Red 52, and Tartrazine cannot be uniformly dispersed at a concentration of 2% or 4% to form a uniform substance, and cannot be dispersed, so it is impossible to Further preparation of colored laundry detergent.
  • the colored washing powder prepared by using the dye dispersion of the present invention can achieve a wider range of color shades, so that the colored washing powder can achieve better color performance.

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Abstract

一种染料分散体，其中包含多元醇以及分散于其中的水溶性染料，相比于其他色料分散体，具有更低的设备沾染性，不易对设备染色、易于清洗，有效提高了染料分散体配方的灵活性，且具有更低的黏度；一种制备彩色洗衣粉的方法，其包含以下步骤：制备染料分散体和将所述染料分散体均匀喷洒在洗衣粉基粉上，且该染料分散体包含多元醇以及分散于其中的水溶性染料，该方法工序可独立于常规洗衣粉的制备流程之外单独设置，同时无需引入的额外的干燥工序以脱去水分；一种染料分散体用于制备彩色洗衣粉的用途以及由所述制备彩色洗衣粉的方法制备得到的彩色洗衣粉。

Description

用于制备彩色洗衣粉的染料分散体及彩色洗衣粉的制备方法 技术领域
本发明涉及洗衣粉制备领域，具体涉及一种用于制备彩色洗衣粉的染料分散体以及使用该染料分散体制备彩色洗衣粉的方法。
背景技术
洗衣粉是日常生活中重要的洗涤剂。伴随消费需求多样化，彩色洗衣粉应运而生。通常的洗衣粉生产流程是将用于织物清洁目的的洗涤剂原料如各类表面活性剂及洗涤助剂类原料混合配制成料浆，通过高塔喷雾经过热风干燥后得到一定密度和粒径的洗衣粉颗粒。为赋予洗衣粉更加丰富的功能以满足多样化需求，在后配阶段还可以混入各种添加剂，如酶，聚合物，香精，非离子表面活性剂等，以丰富产品性能。
本发明涉及的彩色洗衣粉领域中现有的制备工艺通常是前配工艺，即将色素原料与料浆在喷粉工艺之前配制混合，具体而言，该工艺的基本流程为在料浆内添加适当比例的某种色素原料，混合均匀后喷粉造粒得到颜色均匀的彩色洗衣粉颗粒。但这样的生产过程会造成喷粉塔被色素污染，影响后续的洗衣粉生产，如果清洗喷粉塔，同样也是耗时耗力的。
与前配工艺相对的制备工艺被称为后配工艺，也可用于彩色洗衣粉的生产，例如CN110846140A公开了一种彩色洗衣粉的制备工艺，该工艺以非离子表面活性剂来分散染料，在后配过程中雾化喷洒在洗衣粉颗粒表面，该工艺中染料-非离子表活溶液中非离子表面活性剂的含量要求为90-99.5％，这样的含量范围较高，会影响洗衣粉配方中表面活性剂的总含量，特别是当面对洗衣粉基粉配方中要求不添加非离子表面活性剂的情况时，该制备方法的应用将受到严重的限制。
即便如此，后配工艺在彩色洗衣粉制备仍然具备相当明显的优势，原因在于：一方面后配工艺不需要对现有的洗衣粉生产线做大规模的改进，仅需要增加喷洒工序将制备得到的色料分散体喷洒在洗衣粉基粉上；另一 方面，后配工艺赋予了洗衣粉额外的色彩层次以满足个性化需求。但后配工艺的应用目前仍然受到限制，因为其不可避免地在原洗涤颗粒中引入了色料分散体，作为额外添加的成分，染料分散体的引入从整体上改变了洗衣粉的组成。因而在开发前配工艺时，对于色料分散体的选择至关重要，而色料分散体的选择也直接影响到彩色洗衣粉制备方法工艺的设计。
发明内容
本发明提供一种染料分散体，其中包含多元醇以及分散于其中的水溶性染料。
关于用于后配工艺中的彩色分散体的选择，发明人发现：在后配工艺中通过喷洒工序引入的色料分散体，作为洗衣粉中的额外成分，应当尽可能小地影响洗衣粉基粉的组成，这意味着：引入的色料分散体应当在一定重量下尽可能含有更多的色料成分，同时应当能够适应后配工艺对于物料的需求，特别是喷洒工序中对于黏度的要求。
发明人注意到：后配工艺中的喷洒工序是不可避免的，出于节约生产成本的考虑，喷洒装置往往同时用以制备白色的洗衣粉基粉和彩色洗衣粉，因而需要在色料溶液和无色溶液切换使用，这就要求色料溶液不易造成设备染色、易于清洗。
发明人另注意到：后配工艺的优势在于可以通过额外喷洒色料染色的方式制备彩色洗衣粉，因而具备优势，则尽可能适配于目前所有商业化洗衣粉基粉品种，与以各种类型的表面活性剂作为去污活性成分的洗衣粉品种相兼容，这样的综合因素是必须的。
发明人还注意到：后配工艺中水的引入需要在工艺中增加额外的干燥工序，这对于工业生产而言是不利的，因而开发不包含水的染料分散体以及彩色洗衣粉制备方法是有利的。
据此，发明人选取以多元醇作为分散剂的水溶性染料体系作为染料分散体，以克服上述已知的问题。本发明涉及的染料分散体，相比于其他色料分散体，具有更低的设备沾染性，不易对设备染色、易于清洗；多元醇作为分散剂，相比于表面活性剂具有更低的价格，可以有效地提高染料分散体配方的灵活性；另外，相比于表面活性剂，特别是非离子型表面活性 剂，多元醇具有更低的黏度，这对于喷洒工序也是有利的。另外，由于本发明涉及的染料分散体中并不包含水，不必额外引入的干燥工艺，这拓宽了本发明的应用场景。
另外，发明人意外地发现：使用聚合物色素的染料分散体的黏度随着分散体中色料浓度而降低，这使得聚合物色素一方面因其不需要借助表面活性剂开展分散而满足了配方不含表面分散活性剂的条件，另一方面因其浓度越高黏度越低的特性而为低浓度高色料浓度成为可能，因而聚合物色素分散体是在后配工艺制备彩色洗衣粉方面的前景相当广阔。
本发明还提供一种制备彩色洗衣粉的方法，其包含以下步骤：制备染料分散体和将所述染料分散体均匀喷洒在洗衣粉基粉上，且该染料分散体包含多元醇以及分散于其中的水溶性染料。
关于制备彩色洗衣粉的方法的工序及步骤，本发明人发现：喷洒工序中使用的染料分散体配方兼容性强且无沾染设备的风险，该方法工序可独立于常规洗衣粉的制备流程之外单独设置。这极大地拓宽了后配工艺的应用场景。
本发明人发现：如果分散体中并不包含额外的水，在喷洒工序后无需引入的额外的干燥工序以脱去水分，这对工业生产来说是有利的。
基于聚合物色素在聚合物色素分散体方面的应用前景，本发明人发现：使用聚合物色素分散体，特别是聚合物色素-丙二醇分散体可以在工业可接受的条件下实现更优异的表现。
本发明还提供一种染料分散体用于制备彩色洗衣粉的用途以及由本发明所述制备彩色洗衣粉的方法制备得到的彩色洗衣粉。
具体实施方式
本发明中使用的名词术语应本领域一般技术人员的通常理解。为便于理解发明内容的目的，对特定术语的含义描述如下。以下描述无意限缩本发明的保护范围，仅代表发明人在发明做出时对于相关内容的理解。
染料分散体
本发明的染料分散体是将水溶性染料分散于分散介质中形成的均匀物质。
本发明的水溶性染料是色料/着色剂的子集，包括所有能在水中溶解的大分子或小分子着色类物质。
本发明中水溶性染料优选为聚合物色素。聚合物色素是通常是指具有与至少一个低聚或聚合链相连的至少一个发色基团部分的色料，其中所述链具有至少三个重复单元。低聚或聚合成分可经由任何合适的方式结合到发色基团上，诸如通过共价键、离子键或合适的静电相互作用。通常，聚合物色素可特征在于具有介于约300nm和约900nm范围内的吸光度，该吸光度通过紫外-可见光光谱来测量。
由于其生产工艺，聚合物色素的分子量通常表现为分子量分布。因此，聚合物色素的分子量通常报道为通过其分子量分布来确定的平均分子量。
着色剂的发色基团广泛可变，并且可包括该领域中特征为染料或颜料的化合物。所用的实际基团将很大程度上取决于，例如，所需的颜色和颜色牢固度特征。发色基团可通过合适的氮、氧、硫等连接部分而与至少一个聚亚烷氧基(polyalkyleneoxy)取代基相连。
发色基团的例子包括亚硝基、硝基、偶氮(包括单偶氮、二偶氮、三偶氮、四偶氮、多偶氮、甲臜、偶氮甲碱及其金属复合物)、1,2-二苯乙烯、二芳基甲烷、三芳基甲烷、呫吨吖啶、喹啉、次甲基(包括多次甲基)、噻唑、吲达胺、靛酚、吖嗪、噻嗪、噁嗪、氨基酮、羟基酮、蒽醌(包括蒽吡唑啉、蒽酮、蒽吡啶酮、蒽嘧啶、黄烷士酮、皮蒽酮、苯并蒽酮、苝、紫环酮(perinone)、萘二甲酰亚胺及形式上与蒽醌相关的其它结构)、靛青类(包括硫靛)、酞菁发色基团以及它们的混合物。
合适的聚合链的例子是聚亚烷氧基链。本文所用的术语“聚亚烷氧基(polyalkyleneoxy)”通常是指含有以下重复单元的分子结构：-CH 2CH 2O-、CH 2CH 2CH 2O-、-CH 2CH 2CH 2CH 2O-、-CH 2CH(CH 3)O-、-CH 2CH(CH 2CH 3)O-CH 2CH 2CH(CH 3)O-以及它们的任何组合。
这种可与发色基团相连的基团的典型是聚环氧化物，诸如聚环氧烷及其共聚物。可用于提供着色剂的典型的聚环氧烷及其共聚物包括由含有2-20个碳原子、或者更优选2-6个碳原子的环氧烷(烯化氧)单体制成的那些。例子包括：聚环氧乙烷；聚环氧丙烷；聚环氧丁烷；氧杂环丁烷(oxetanes)；四氢呋喃；聚环氧乙烷、聚环氧丙烷和聚环氧丁烷的共聚物；以及包含嵌 段共聚物的其它共聚物，其中大部分聚合取代基为聚环氧乙烷、聚环氧丙烷和/或聚环氧丁烷。另外，这种聚亚烷氧基基团的平均分子量可在约132到约10,000、优选176到约5000的范围内。
应理解由于着色剂通常可以不与载体化学结合，因此只要着色剂的正确功能与组成相关，聚亚烷氧基基团上的末端基团的精确化学本体可能不太关键。考虑到这点，某些最优选的着色剂将被确定，其中确认了某些末端基团。这种关于末端基团的陈述并非理解为以任何方式将本发明限制在其较宽的实施方式中。根据这样的最优选实施方式，着色剂特征可在于以下：
R{A[(亚烷氧基成分) nR 1] m} x
其中R是有机发色基团，A是所述有机发色基团中连接部分且选自N、O、S或CO 2，所述亚烷氧基成分的亚烷基部分包含约2到约4个碳原子，n是2到约230的整数，当A是O、S、CO 2时m为1，且当A是N时m为1或2，x是1到5的整数，且n乘x乘m(n.m.x)的积为2到约230，且R 1是选自以下的一员：
Figure PCTCN2022131024-appb-000001
以及所述组中每个成员的磺酸盐和硫酸盐，其中R 2是H、含有最多约20个碳原子的烷基或含有最多约20个碳原子的羧基封端的烷基，j和k是OH、OM或OR 3，其中M是碱金属、碱土金属、过渡金属(例如镍等)或铵的阳离子部分，且R 3是含有最多约20个碳原子的烷基。
低聚成分可以是任何合适的成分，包括但不限于选自以下的低聚成分：(i)包含最少三个选自C 2-C 20亚烷氧基基团、缩水甘油(glycidol)基团和缩水甘油基(glycidyl)基团的单体或重复单元的低聚物，(ii)符合结构(I)的芳族或脂族低聚酯：
Figure PCTCN2022131024-appb-000002
以及(iii)(i)和(ii)的组合。在结构(I)，R 2和R 3独立地选自氢和C 1-C 10烷基，f是介于1到10之间的整数并且包括1和10，且g是介于1到20之间并包括1和20的任何正整数或分数。本领域技术人员应理解，g的合适值既包括整数也包括分数，这是因为单个聚合物色素分子上的低聚成分的长度可变。因此，对于指定的聚合物色素分子样品或集合来说，g的值代表酯链的平均长度。在某些实施方式中，聚合物色素可包括一个或更多个由三个或更多个环氧乙烷单体基团组成的低聚成分。
示例性的聚合物色素包括
Figure PCTCN2022131024-appb-000003
聚合物色素和
Figure PCTCN2022131024-appb-000004
聚合物色素，其中聚合物色素
Figure PCTCN2022131024-appb-000005
是更为优选的。
所有这些聚合物色素可从美利肯化学公司得到，该公司是位于南卡罗来纳州斯巴达堡的美利肯公司的分公司。
Figure PCTCN2022131024-appb-000006
聚合物色素的特征在于它们是水溶性的、不染色的着色剂。它们广泛用于衣物洗涤剂、织物柔软剂以及其它消费和工业清洁产品中。
Figure PCTCN2022131024-appb-000007
聚合物色素通常为光亮的液体着色剂，其在水中显示极好的溶解性，与其终端用途配方中存在的其它化学品相容，并且易于处理。
Figure PCTCN2022131024-appb-000008
聚合物色素可用于在水性和固体系统中提供颜色。
Figure PCTCN2022131024-appb-000009
聚合物色素的独特的聚合特性提供了对皮肤、纺织品、硬表面、设备等的较低染色。
Figure PCTCN2022131024-appb-000010
聚合物色素是特别开发用于可洗涤用途的液体着色剂，诸如用于标记物、油漆和其它艺术产品中。它们不包含重金属，无毒，并且在皮肤、织物和其它表面上具有极好的不染色性质。
Figure PCTCN2022131024-appb-000011
聚合物色素具有与水性油墨制品的极好相容性，并且提供鲜艳的颜色。
本发明范围内的染料还可以是选自以下类别中的一种或多种的着色剂可适合用作色粒中的着色剂：酸性染料、碱性染料、直接染料、溶剂染料、还原染料、媒染料、靛类染料、活性染料、分散染料、硫化染料、荧光染料、天然着色剂等。
在本发明的一些实施方式中，水溶性染料在染料分散体中的重量百分 比为0-95％，上述重量百分比以染料分散体的总重量计。在一些优选的实施方式中，水溶性染料在分散体的中的重量百分5-40％，更优选为10-20％。该含量范围赋予染料分散体宽泛的色彩范围，使得由该染料分散体制备得到的彩色洗衣粉在颜色浓度上具有更宽的选择范围，同时兼顾了染料分散体黏度的平衡，适用于后配工艺中的喷洒工序。
本发明中选用多元醇作为分散剂以分散水溶性染料。多元醇优选的实例包括丙二醇和甘油。多元醇的添加量或者其在染料分散体中的百分含量是依据选择的水溶性染料确定的。当选用溶解范围较宽的水溶性染料时，分散剂的含量范围可以更大。
发明人已经发现控制上述染料分散体的黏度对于喷洒工序乃至整个彩色洗衣粉生产后配工艺是重要的，综合染色表现以及分散体浓度等多方面因素，发明人发现不超过80mPa.s的黏度范围是优选的，兼顾染料分散体中色料浓度、喷洒工艺的要求以及温度对黏度的影响等影响，优选不超过60mPa.s，特别优选10～60mPa.s；对于聚合物色素分散体而言，进一步优选的黏度范围为20～40mPa.s。
在本发明的一种实施方式中，所述染料分散体中不包含表面活性剂或水。上述排除性限定的原因是，本发明人发现多元醇对于水溶性染料具有良好的分散表现，此种情况下无需再加入表面活性剂或水以提高分散体系的分散度，并赋予染料分散体更好的配方灵活性。
在发明的一种优选实施方式中，所述染料分散体为黏度为10-60mPa.s的聚合物色素-丙二醇分散体，其中聚合物色素的重量百分比为0.01～40％。
彩色洗衣粉制备方法
本发明中制备彩色洗衣粉方法包括制备如上文描述的染料分散体，并将该染料分散体均匀喷洒在洗衣粉基粉上。其中洗衣粉基粉及其制备方法、制备本发明中染料分散体中涉及的操作步骤与工序是本领域的已知的。将染料分散体均匀喷洒于基粉上的方法了涵盖使用工业喷嘴、雾化器及其他分散设备，将液态分散体涂布与洗衣粉基粉粉体外侧的方式。
基于发明人发现本发明的染料分散体具有上述特点，特别是在良好的色彩表现以及黏度间实现了优异的平衡，开发出了本发明中制备彩色洗衣粉的方法。
在本发明的一种实施方式中，因为所使用的染料分散体中不包含水或表面活性剂，因而在将该染料分散体均匀喷洒在洗衣粉基粉上后无需额外的干燥工序以脱去水分，简化了工序，有效降低了工业生产的成本。
在本发明的一种优选实施方式中，使用的染料分散体为黏度为10-60mPa.s的聚合物色素-丙二醇分散体，其中聚合物色素的重量百分比为0.01～40％。
实施例
下述实施例用以阐明本发明的内容以进一步理解本发明。这些实施例无意以任何方式限制本发明的保护范围。
实验I：染料分散体的制备
按表1中重量百分比配制足量染料分散体，待用。
Figure PCTCN2022131024-appb-000012
Figure PCTCN2022131024-appb-000013
表1：实施例与对比例的染料分散体制备组成
A1、A3、A5、A7、A9以及A11均为以丙二醇为分散介质的染料分散体。制备过程中，耐晒翠兰(FBL)、酸性红52、柠檬黄等水溶性染料在20％或40％的浓度下分散性差，水溶性染料混合物在制备过程中呈现膏状，故将传统水溶性染料的浓度相应调整为2％或4％；但在20％甚至40％的重量百分比下，
Figure PCTCN2022131024-appb-000014
聚合物色素分散表现良好。
B1、B3、B5、B7、B9以及B11均为以AOE9(一种可商购的非离子型表面活性剂)为分散介质的染料分散体。耐晒翠兰(FBL)、酸性红52、柠檬黄等水溶性染料在2％或4％的浓度下已经无法均匀分散进而形成均一的物质，表现出无法接受的分散性能；但在20％和40％的重量百分比下，
Figure PCTCN2022131024-appb-000015
聚合物色素分散性表现良好。
实验II：染料分散体的性能评价
II-1.传统水溶性染料分散体与聚合物色素分散体的黏度对比测试
在室温条件下，配制5％浓度的不同染料的丙二醇分散体，测试其黏度后汇总数据如表2所示。
Figure PCTCN2022131024-appb-000016
表2：5％浓度下几种传统水溶性染料-丙二醇分散体与聚合物色素-丙二醇分散体浓度对比
传统水溶性染料分散体在6％的浓度下已经不能很好分散于丙二醇中，因而选择传统水溶性染料能够分散的极限浓度作为黏度测试浓度。由上表可知，在5％的浓度下，所有颜色的
Figure PCTCN2022131024-appb-000017
-丙二醇分散体都表现出了显著更低的黏度，而黏度增加会增加化工生产中传质单元推进力负担，增加化工过程能源消耗，不利于生产。因而
Figure PCTCN2022131024-appb-000018
相较于传统水溶性染料在后配工艺中更具潜力。
II-2.不同浓度下聚合物色素分散体的黏度对比测试
分别配制重量百分比为5％、10％、20％和40％的不同
Figure PCTCN2022131024-appb-000019
-丙二醇分散体，测试其黏度后汇总数据如表3所示。
Figure PCTCN2022131024-appb-000020
表3：不同浓度下几种
Figure PCTCN2022131024-appb-000021
-丙二醇分散体黏度数据
在每一种
Figure PCTCN2022131024-appb-000022
聚合物色素-丙二醇分散体中，分散体黏度都随着聚合物色素浓度增加而降低。当聚合物色素浓度达到40％时，分散体黏度下降至20mPa.s左右。将浓度的变化趋势和温度对于物质黏度的影响纳入考量因素，0.01％～40％的浓度下，聚合物色素分散体的黏度范围为10～60mPa.s。
考虑到聚合物色素在丙二醇及其他多元醇中卓越的分散表现，以及伴随着浓度升高表现出的黏度降低，使得在通过后配工艺制备彩色洗衣粉时，
Figure PCTCN2022131024-appb-000023
聚合物色素能够在帮助彩色洗衣粉提高色彩表现的同时，降低喷洒用色料分散体的黏度。这对于提升彩色洗衣粉的质量并降低工业生产成本都是有利的。
II-3.染料分散体的设备沾染性
(1)取A5、A6、A9以及A10四组分散体各2ml，分别滴在四个光洁的304不锈钢托盘上；
(2)静置过夜；
(3)使用清水和软布清洗并擦拭四个不锈钢托盘，观察金属表面的外观变化。
比较A5、A6、A9以及A10四组分散体承托与于不锈钢托盘时的染色情况，A6承载A6和A10的托盘在清洗后光洁如初，承载A9的托盘残留 轻微的黄色，承载A5存在较为明显的颜色改变。
可见，A6和A10所对应的
Figure PCTCN2022131024-appb-000024
聚合物色素染料分散体具有更低的设备沾染性和设备损害性。
实验III：彩色洗衣粉制备与色彩评价
III-1.彩色洗衣粉的制备
(1)根据表4示出配方分别制备500g彩色洗衣粉，其中使用的染料分散体为本发明中涉及的染料分散体A1～A12(使用的洗衣粉基粉为市售产品)；
Figure PCTCN2022131024-appb-000025
表4：实施例的彩色洗衣粉制备组成
(2)称取相应重量的洗衣粉置于旋转包衣装置内，开启转鼓，调至40-50RPM匀速旋转，并按需称取相应质量密封待用；
(3)在实验室条件下，将相应的染料分散体以0.20MPa的压力进行高压雾化，喷洒至旋转混合器中的洗衣粉基粉中，然后在旋转混合器中充分混合；
(4)共制得C1～C12的彩色洗衣粉各500g，封罐待用。
鉴于采用AEO9作为分散介质时，晒翠兰(FBL)、酸性红52、柠檬黄等水溶性染料在2％或4％的浓度下已经无法均匀分散进而形成均一的物质，无法分撒，因而无法进一步制备彩色洗衣粉。
III-2.彩色洗衣粉的色彩表现评价
比较C1、C2、C3以及C4四组彩色洗衣粉的色彩表现，可以发现C2 和C4相比于C1和C3表现出了明显更深的蓝色；即使是染料分散体使用量更低的C4(2.5g)相较于染料分散体使用量更高的A1(5g)也具有明显可感的更深的蓝色。
可见，在使用相同质量的染料分散体时，使用本发明的染料分散体制备得到的彩色洗衣粉可以实现更宽泛的色彩深浅范围，使得彩色洗衣粉取得更优异的色彩表现。

Claims (10)

  1. 一种用于制备彩色洗衣粉的染料分散体，其特征在于：包含多元醇以及分散于其中的水溶性染料，其中水溶性染料的重量百分比为0.01～40％，所述染料分散体的黏度为10～60mPa.s。
  2. 根据权利要求1所述的染料分散体，其特征在于：所述染料分散体中表面活性剂含量小于1％。
  3. 根据权利要求1所述的染料分散体，其特征在于：所述多元为丙二醇或甘油。
  4. 根据权利要求1所述的染料分散体，其特征在于：所述多元醇为丙二醇或甘油，表面活性剂含量小于1％,所述水溶性染料为聚合物色素，其中聚合物色素的重量百分比为5～40％，所述染料分散体的黏度为20～40mPa.s。
  5. 根据权利要求1～4中任意一项所述的染料分散体用于制备彩色洗衣粉的用途。
  6. 一种制备彩色洗衣粉的方法，其特征在于包含以下步骤：
    (1)制备染料分散体；
    (2)将所述染料分散体均匀喷洒在洗衣粉基粉上；
    其中，所述染料分散体中水溶性染料的重量百分比为0.01～40％，所述染料分散体的黏度为10～60mPa.s。
  7. 根据权利要求6所述的方法，其特征在于：所述染料分散体中表面活性剂含量小于1％。
  8. 根据权利要求6所述的方法，其特征在于：所述多元醇为丙二醇或甘油，表面活性剂含量小于1％,所述水溶性染料为聚合物色素，其中聚合物色素的重量百分比为5～40％，所述染料分散体的黏度为20～40mPa.s。
  9. 根据权利要求6所述的方法，其特征在于：在步骤(2)之后不包含额外的干燥工序以脱去水分。
  10. 由权利要求6～9中任意一项所述的方法制得的彩色洗衣粉。
PCT/CN2022/131024 2021-11-11 2022-11-10 用于制备彩色洗衣粉的染料分散体及彩色洗衣粉的制备方法 WO2023083238A1 (zh)

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US4150947A (en) * 1968-03-01 1979-04-24 Ciba-Geigy Ag Stable, concentrated dispersions of basic dyestuffs
GB1513526A (en) * 1977-01-20 1978-06-07 Ici Ltd Dye dispersions
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