阅读说明：本技术 一种用于生产洗涤剂的脂肪酸甲酯磺酸钠组合物粒子 (Sodium fatty acid methyl ester sulfonate composition particles for producing detergent ) 是由 蒋良宇 李春霞 杨天奎 于 2019-11-27 设计创作，主要内容包括：本发明提供一种用于生产洗衣粉的脂肪酸甲酯磺酸钠(MES)组合物粒子及其制备方法。本发明的MES组合物粒子含有20～65质量份的脂肪酸甲酯磺酸钠、10～35质量份的纯碱、0.05～5质量份的羧甲基纤维素钠、5～65质量份的硫酸钠、0.1～10质量份的聚合物和0～15质量份的泡花碱。本发明解决了洗衣粉生产过程中MES在高温、强碱性体系中水解,MES在使用时稳定性差、刺激性大、易分解和易结块,MES在低温下溶解速度慢,和洗衣粉中MES含量低的问题。(The invention provides a fatty acid methyl ester sodium sulfonate (MES) composition particle for producing washing powder and a preparation method thereof. The MES composition particles comprise 20-65 parts by mass of fatty acid methyl ester sodium sulfonate, 10-35 parts by mass of soda ash, 0.05-5 parts by mass of sodium carboxymethyl cellulose, 5-65 parts by mass of sodium sulfate, 0.1-10 parts by mass of a polymer and 0-15 parts by mass of sodium silicate. The invention solves the problems that MES is hydrolyzed in a high-temperature and strong-alkaline system in the production process of the washing powder, MES is poor in stability, large in irritation, easy to decompose and agglomerate when used, MES is low in dissolving speed at low temperature, and MES content in the washing powder is low.)

1. A sodium fatty acid methyl ester sulfonate composition particle, characterized in that the sodium fatty acid methyl ester sulfonate composition particle contains 20-65 parts by mass of sodium fatty acid methyl ester sulfonate, 10-35 parts by mass of soda ash, 0.05-5 parts by mass of sodium carboxymethylcellulose and 5-65 parts by mass of sodium sulfate, and per 100 parts by mass of sodium fatty acid methyl ester sulfonate, soda ash, sodium carboxymethylcellulose and sodium sulfate, 0.1-10 parts by mass of a polymer and 0-15 parts by mass of sodium silicate; preferably, the sodium fatty acid methyl ester sulfonate composition particles do not contain zeolite.

2. The sodium fatty acid methyl ester sulfonate composition particles of claim 1,

the carbon atom number of long-chain alkyl in the fatty acid methyl ester sodium sulfonate is 12-18; and/or

The polymer is one or the combination of any more of acrylic acid homopolymer, maleic acid-acrylic acid copolymer and acrylic acid-styrene copolymer; and/or

The particle size of the fatty acid methyl ester sodium sulfonate composition particles is less than or equal to 1.3 mm.

3. The sodium fatty acid methyl ester sulfonate composition particles of claim 1 or 2, wherein in the sodium fatty acid methyl ester sulfonate composition particles,

the content of the fatty acid methyl ester sodium sulfonate is 30-60 parts by mass; and/or

The content of the soda ash is 15-30 parts by mass; and/or

The content of the sodium carboxymethylcellulose is 0.1-3 parts by mass; and/or

The content of sodium sulfate is 5-50 parts by mass; and/or

The content of the polymer is 0.5-6 parts by mass per 100 parts by mass of fatty acid methyl ester sodium sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate; and/or

The content of sodium silicate is 0-8 parts by mass per 100 parts by mass of fatty acid methyl ester sodium sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate.

4. A method for preparing sodium fatty acid methyl ester sulfonate composition particles, the method comprising:

(1) dissolving a polymer and optionally a sodium silicate in a binder to obtain a liquid containing the polymer, optionally the sodium silicate and the binder;

(2) contacting a solid mixture containing 20-65 parts by mass of sodium fatty acid methyl ester sulfonate, 10-35 parts by mass of sodium carbonate, 0.05-5 parts by mass of sodium carboxymethylcellulose and 5-65 parts by mass of sodium sulfate with the liquid containing the polymer, optional sodium silicate and a binder obtained in the step (1) in a fluidized bed, granulating in the fluidized bed, and drying after the granulation is finished; wherein the solid mixture and the liquid containing the polymer, the optional sodium silicate and the adhesive are used in the following ratio: the dosage of the polymer is 0.1-10 parts by mass of each 100 parts by mass of fatty acid methyl ester sodium sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate, and the dosage of the sodium silicate is 0-15 parts by mass of each 100 parts by mass of fatty acid methyl ester sodium sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate;

preferably, the solid mixture in a fluidized state is contacted with the atomized liquid containing polymer, optionally sodium silicate and binder.

5. The method of claim 4,

the adhesive is one or the combination of any more of water, alcohol, propylene glycol and glycerol; and/or

The carbon atom number of long-chain alkyl in the fatty acid methyl ester sodium sulfonate is 12-18; and/or

The polymer is one or the combination of any more of acrylic acid homopolymer, maleic acid-acrylic acid copolymer and acrylic acid-styrene copolymer; and/or

The particle size of the fatty acid methyl ester sodium sulfonate composition particles is less than or equal to 1.3 mm.

6. The method of claim 4 or 5,

in the solid mixture, the content of the fatty acid methyl ester sodium sulfonate is 30-60 parts by mass; and/or

In the solid mixture, the content of the sodium carbonate is 15-30 parts by mass; and/or

In the solid mixture, the content of the sodium carboxymethylcellulose is 0.1-3 parts by mass; and/or

In the solid mixture, the content of sodium sulfate is 5-50 parts by mass; and/or

The dosage of the polymer is 0.5-6 parts by mass of fatty acid methyl ester sodium sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate per 100 parts by mass; and/or

The dosage of sodium silicate is 0-8 parts by mass of sodium fatty acid methyl ester sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate per 100 parts by mass; and/or

The amount of the binder is 5 to 75 parts by mass, preferably 20 to 60 parts by mass, per 100 parts by mass of the fatty acid methyl ester sodium sulfonate, the sodium carbonate, the sodium carboxymethylcellulose and the sodium sulfate.

7. The method of claim 4 or 5,

the sodium fatty acid methyl ester sulfonate, the sodium carbonate, the sodium carboxymethylcellulose and the sodium sulfate are powder with the particle size of less than or equal to 0.20mm, preferably less than or equal to 0.10 mm; and/or

During granulation, air is fed from the bottom of the fluidized bed, the temperature of the air is-10-60 ℃, the preferred temperature is 10-50 ℃, and the relative humidity is 20-80%, the preferred temperature is 30-60%; and/or

The method also comprises the step of sieving after drying, wherein the sieved sieve mesh number is 150 meshes.

8. Sodium fatty acid methyl ester sulfonate composition particles prepared by the process of any one of claims 4 to 7.

9. Use of the sodium fatty acid methyl ester sulfonate composition particles of any one of claims 1 to 3 and 8 in the preparation of a detergent, or in a wash.

10. A detergent comprising the sodium fatty acid methyl ester sulfonate composition particles of any one of claims 1 to 3 and 8; preferably, the detergent is a laundry powder.

Technical Field

The invention relates to the field of household chemicals, in particular to MES composition particles for producing detergents.

Background

The fatty acid methyl ester sodium sulfonate (MES) is an anionic surfactant with excellent performance prepared by adopting natural renewable resources of coconut oil, palm oil and the like, has the advantages of safety, no toxicity, strong hard water resistance and complete biodegradation, is called as a real environment-friendly green surfactant, has equivalent advantages in performance compared with the currently used petroleum-based surfactants (such as sodium dodecyl benzene sulfonate, alpha-sodium alkenyl sulfonate and the like), and has important significance for solving the common problem that the daily chemical industry depends on petroleum for a long time, so the MES gradually becomes a hotspot in the research field of detergents at home and abroad.

However, MES is not resistant to strong alkali, is easily hydrolyzed in a strongly alkaline aqueous solution to generate disodium salt, and MES is not resistant to high temperature, and is easily softened, sticky or even melted under a high-temperature condition. The application difficulty of MES is determined by the characteristics of MES, the MES is less applied to washing powder, and particularly, the preparation of washing powder products with high MES content is blank.

In the traditional washing powder production process, if MES is directly applied to a pre-dosing process, MES is easily decomposed in alkaline washing powder slurry through high-temperature spraying to generate disodium salt to influence the product performance, and MES has certain influence on the rheological property of the washing powder slurry, so that the spraying process is difficult to control. If MES is applied to a washing powder post-preparation process, the performance of the MES in the washing powder is difficult to guarantee, even though the decomposition of MES brought by high temperature, strong alkalinity and aqueous solution to produce disodium salt is avoided, MES can only be used as an auxiliary surfactant to be added into a washing powder formula, the content of MES is only 3-15%, if too much MES is added, great negative effects can be brought to the product performance, such as excessive fine powder, high irritation, nose choking, easy caking of the product in the storage process, poor solubility caused by easy formation of fish eyes when the product is dissolved in water, and the like, and the washing powder with high MES content cannot be prepared in a post-preparation mode. In a word, the direct application of the MES raw material to the washing powder product affects the quality and the performance of the product, which seriously restricts the application of the MES in the washing powder.

Aiming at the problems, if MES composition particles can be prepared and then added into washing powder to obtain a washing powder product with good performance, the MES can be greatly promoted to be applied to the washing powder.

Chinese patent application CN101735892A discloses MES-containing compositions for use in the production of laundry powder which are mixed in a mixer from soda ash, MES, aqueous solutions etc. but such highly alkaline water systems will cause a large amount of MES to be hydrolyzed into disodium salts, affecting the product performance, and furthermore the solubility of the particles is seriously questionable by preparing the wet MES-containing compositions into particles by means of an oscillating granulator. The Chinese patent application CN102277238A discloses a granular MES-containing composition, and the method utilizes an extrusion granulation process, and the extruded and granulated particles have higher density, poorer solubility and particularly poorer low-temperature solubility. Chinese patent application CN101955855A discloses a spherical detergent composition and its manufacturing method, which utilizes wet mixture, and extrudes into thin strips through an extruder, and then pelletizes into spherical particles through a spheronization pelletizer. Chinese patent application CN102994258A discloses a method for preparing a detergent composition containing MES, wherein a nonionic surfactant is sprayed on powdered MES in a spraying manner to form a nonionic film wrapping layer on the surface of the MES, compared with the powdered MES, the flowability of the composition is improved to a certain extent, but the flowability is still poor, in addition, the nonionic surfactant is easy to form gel, so that the solubility of the composition in water is poor, and therefore the solubility in water is seriously questionable, and the properties of caking resistance, particle size distribution, particle compressive strength and the like of the composition prepared in a drum mixer in a spraying manner are seriously questionable.

In addition, zeolite is added into the MES composition as a filler, the zeolite has a unique pore structure, a plurality of cavities are formed in the middle of the zeolite, water easily enters the cavities of the zeolite when the MES composition is dissolved, and the dissolution of MES can be accelerated.

In order to better utilize MES materials and solve the disadvantages of the prior art, there is still a need in the art for novel MES composition particles.

Disclosure of Invention

The invention provides a sodium fatty acid methyl ester sulfonate composition particle for producing a detergent, which aims to solve the problem of application of sodium fatty acid methyl ester sulfonate in a detergent, especially a washing powder, and comprises 20-65 parts by mass of sodium fatty acid methyl ester sulfonate, 10-35 parts by mass of soda ash, 0.05-5 parts by mass of sodium carboxymethylcellulose and 5-65 parts by mass of sodium sulfate, and 0.1-10 parts by mass of a polymer and 0-15 parts by mass of sodium silicate, the soda ash, the sodium carboxymethylcellulose and the sodium sulfate are counted by 100 parts by mass in total.

In one or more embodiments, the number of carbon atoms in the long chain alkyl group in the sodium fatty acid methyl ester sulfonate is 12 to 18.

In one or more embodiments, the polymer is one or a combination of any of an acrylic acid homopolymer, a maleic acid-acrylic acid copolymer, and an acrylic acid-styrene copolymer.

In one or more embodiments, the particles of the sodium fatty acid methyl ester sulfonate composition have a particle size of ≦ 1.3mm, preferably 0.1 to 1.3 mm.

In one or more embodiments, the sodium fatty acid methyl ester sulfonate composition particles do not contain zeolites.

In one or more embodiments, the content of the sodium fatty acid methyl ester sulfonate in the particles of the sodium fatty acid methyl ester sulfonate composition is 30 to 60 parts by mass.

In one or more embodiments, the sodium fatty acid methyl ester sulfonate composition particles have a content of sodium carbonate of 15 to 30 parts by mass.

In one or more embodiments, the sodium fatty acid methyl ester sulfonate composition particles contain sodium carboxymethylcellulose in an amount of 0.1 to 3 parts by mass.

In one or more embodiments, the sodium fatty acid methyl ester sulfonate composition particles have a sodium sulfate content of 5 to 50 parts by mass.

In one or more embodiments, the content of the polymer in the particles of the sodium fatty acid methyl ester sulfonate composition is 0.5 to 6 parts by mass per 100 parts by mass of sodium fatty acid methyl ester sulfonate, soda ash, sodium carboxymethyl cellulose, and sodium sulfate.

In one or more embodiments, the sodium fatty acid methyl ester sulfonate composition particles contain sodium salt of sodium methyl ester sulfonate, soda ash, sodium carboxymethylcellulose, and sodium sulfate in an amount of 0 to 8 parts by mass per 100 parts by mass of the sodium fatty acid methyl ester sulfonate, sodium carbonate, and sodium carboxymethylcellulose.

The invention also provides a method for preparing the sodium fatty acid methyl ester sulfonate composition particles by adopting the fluidized bed, which comprises the following steps:

(1) dissolving a polymer and optionally a sodium silicate in a binder to obtain a liquid containing the polymer, optionally the sodium silicate and the binder;

(2) and (2) contacting a solid mixture containing 20-65 parts by mass of sodium fatty acid methyl ester sulfonate, 10-35 parts by mass of sodium carbonate, 0.05-5 parts by mass of sodium carboxymethylcellulose and 5-65 parts by mass of sodium sulfate with the liquid containing the polymer, optional sodium silicate and the binder obtained in the step (1) in a fluidized bed, granulating in the fluidized bed, and drying after the granulation is finished.

In one or more method embodiments, the solid mixture in a fluidized state is contacted with the atomized liquid comprising polymer, optionally sodium silicate, and binder in a fluidized bed.

In one or more method embodiments, the solid mixture and the liquid containing the polymer, optional sodium silicate, and binder are present in an amount ratio that: the dosage of the polymer is 0.1-10 parts by mass per 100 parts by mass of fatty acid methyl ester sodium sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate, and the dosage of the sodium silicate is 0-15 parts by mass per 100 parts by mass of fatty acid methyl ester sodium sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate.

In one or more method embodiments, the binder is one or a combination of any of water, alcohol, propylene glycol, and glycerin.

In one or more embodiments of the method, the number of carbon atoms in the long chain alkyl group in the sodium fatty acid methyl ester sulfonate is 12 to 18.

In one or more embodiments of the method, the polymer is one or a combination of any of an acrylic acid homopolymer, a maleic acid-acrylic acid copolymer, and an acrylic acid-styrene copolymer.

In one or more method embodiments, the particles of the sodium fatty acid methyl ester sulfonate composition have a particle size of 1.3mm or less.

In one or more method embodiments, the sodium fatty acid methyl ester sulfonate, soda ash, sodium carboxymethyl cellulose and/or sodium sulfate are powders having a particle size of 0.20mm or less, preferably 0.10mm or less.

In one or more embodiments of the process, air is introduced from the bottom of the fluidized bed at a temperature of-10 ℃ to 60 ℃, preferably 10 ℃ to 50 ℃, and a relative humidity of 20% to 80%, preferably 30% to 60%, during granulation.

In one or more method embodiments, the method further comprises, after drying, sieving through a sieve having a mesh size of 150 mesh.

In one or more embodiments of the method, the content of the sodium fatty acid methyl ester sulfonate in the solid mixture is 30 to 60 parts by mass.

In one or more method embodiments, the content of soda ash in the solid mixture is 15 to 30 parts by mass.

In one or more method embodiments, the amount of sodium carboxymethylcellulose in the solid mixture is 0.1 to 3 parts by mass.

In one or more method embodiments, the sodium sulfate is present in the solid mixture in an amount of 5 to 50 parts by mass.

In one or more method embodiments, the solid mixture and the liquid containing the polymer, optional sodium silicate, and binder are present in an amount ratio that: the amount of the polymer is 0.5 to 6 parts by mass per 100 parts by mass of sodium fatty acid methyl ester sulfonate, soda ash, sodium carboxymethylcellulose and sodium sulfate.

In one or more method embodiments, the solid mixture and the liquid containing the polymer, optional sodium silicate, and binder are present in an amount ratio that: the dosage of sodium silicate is 0-8 parts by mass of sodium fatty acid methyl ester sulfonate, sodium carbonate, sodium carboxymethylcellulose and sodium sulfate per 100 parts by mass.

In one or more method embodiments, the solid mixture and the liquid containing the polymer, optional sodium silicate, and binder are present in an amount ratio that: the amount of the binder is 5 to 75 parts by mass, preferably 20 to 60 parts by mass, per 100 parts by mass of the fatty acid methyl ester sodium sulfonate, the sodium carbonate, the sodium carboxymethylcellulose and the sodium sulfate.

The invention also provides the particles of the fatty acid methyl ester sodium sulfonate composition prepared by the preparation method of any embodiment of the invention.

The invention also provides the application of the sodium fatty acid methyl ester sulfonate composition particles in any embodiment of the invention in preparing detergents, especially washing powder, or in washing.

The invention also provides a detergent containing the sodium fatty acid methyl ester sulfonate composition particles according to any embodiment of the invention; preferably, the detergent is a laundry powder.

Drawings

FIG. 1 is a schematic structural diagram of a fluidized bed granulator used for preparing sodium fatty acid methyl ester sulfonate composition particles.

The reference numerals are explained below: 1-a fluidized bed body; 2-a spraying device; 3-a dust removal device; 4-an exhaust fan; 5-compressing air; 6-liquid conveying device; 7-a blower; 8-an air filter; 9-a heater.

Detailed Description

To make the features and effects of the present invention comprehensible to those skilled in the art, general description and definitions are made below with reference to terms and expressions mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.

All features defined herein as numerical ranges or percentage ranges, such as numbers, amounts, levels and concentrations, are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range.

In this context, for the sake of brevity, not all possible combinations of features in the various embodiments or examples are described. Therefore, the respective features in the respective embodiments or examples may be arbitrarily combined as long as there is no contradiction between the combinations of the features, and all the possible combinations should be considered as the scope of the present specification.

As used herein, the terms "comprising," "including," or "containing" mean that the various ingredients can be used together in a mixture or composition of the invention. Thus, the terms "consisting essentially of … …" and "consisting of … …" are encompassed by the terms "comprising," including, "or" containing.

The characteristics of raw materials of fatty acid methyl ester sodium sulfonate (MES) determine that MES is easy to hydrolyze in a high-temperature, strong-alkalinity and high-water-content system to generate disodium salt, so that the performance of MES is reduced, and the MES is the most fundamental reason for being incapable of being added into slurry to prepare washing powder. MES in the MES composition particles has stable performance in the preparation process and is not easy to hydrolyze to generate disodium salt. The MES composition particles have the characteristics of no nose choking, uniform particle size, moderate compactness, good solubility and good fluidity, are stable in performance, are not easy to agglomerate and are not easy to break in the storage process, and the problems of poor stability, high irritation, easy decomposition, easy agglomeration and the like of MES in use are solved.

The MES composition particles of the invention comprise MES, soda ash, sodium carboxymethylcellulose, sodium sulfate, a polymer, and optionally sodium silicate. In some embodiments, MES composition particles of the invention consist of MES, soda ash, sodium carboxymethyl cellulose, sodium sulfate, a polymer, and optionally sodium silicate.

MES has the structure shown below:

wherein R is long-chain alkyl. The meaning of the long chain alkyl group in MES is known in the art and refers to an alkyl group having 12 to 20 carbon atoms.

In certain embodiments, the invention uses MES with long chain alkyl groups having 12 to 18 carbon atoms.

The MES composition particles of the present invention contain 20 to 65 parts by mass of MES, for example, 20 to 60 parts by mass, 30 to 60 parts by mass, 35 to 55 parts by mass, and the like.

In the invention, the soda ash can be one or two of light sodium carbonate or heavy sodium carbonate. The MES composition particles of the present invention contain 10 to 35 parts by mass of soda ash, for example, 10 to 30 parts by mass, 15 to 30 parts by mass, 10 to 25 parts by mass, 15 to 25 parts by mass, and the like.

The MES composition particles of the present invention contain 0.05 to 5 parts by mass of sodium carboxymethylcellulose, for example, 0.1 to 5 parts by mass, 0.1 to 3 parts by mass, 0.5 to 2.5 parts by mass, 0.5 to 2 parts by mass, and the like.

The MES composition particles of the present invention contain 5 to 65 parts by mass of sodium sulfate, for example, 5 to 60 parts by mass, 5 to 50 parts by mass, 8 to 45 parts by mass, 20 to 45 parts by mass, and the like.

The MES composition particles of the present invention comprise 20 to 65 parts by mass (for example, 20 to 60 parts by mass, 30 to 60 parts by mass, 35 to 55 parts by mass) of sodium fatty acid methyl ester sulfonate, 10 to 35 parts by mass (for example, 10 to 30 parts by mass, 15 to 30 parts by mass, 10 to 25 parts by mass, 15 to 25 parts by mass) of soda, 0.05 to 5 parts by mass (for example, 0.1 to 5 parts by mass, 0.1 to 3 parts by mass, 0.5 to 2.5 parts by mass, 0.5 to 2 parts by mass) of sodium carboxymethylcellulose, and 5 to 65 parts by mass (5 to 60 parts by mass, 5 to 50 parts by mass, 8 to 45 parts by mass, 20 to 45 parts by mass) of sodium sulfate.

In the MES composition particles of the present invention, the sum of the parts by mass of MES, soda ash, sodium carboxymethylcellulose, and sodium sulfate is usually 100 parts by mass.

Polymers suitable for use in the present invention include, but are not limited to, one or a combination of any of acrylic acid homopolymers, maleic acid-acrylic acid copolymers, and acrylic acid-styrene copolymers. In general, the MES composition particles of the present invention contain 0.1 to 10 parts by mass, for example, 0.1 to 7.5 parts by mass, 0.5 to 6 parts by mass, 0.5 to 5 parts by mass, or the like of a polymer per 100 parts by mass of MES, soda ash, sodium carboxymethylcellulose, and sodium sulfate in total.

In general, the MES composition particles of the present invention contain sodium silicate in an amount or content of 0 to 15 parts by mass, for example, 0 to 8 parts by mass, 0 to 5 parts by mass, 0.1 to 8 parts by mass, 0.1 to 5 parts by mass, or the like, based on 100 parts by mass of MES, soda ash, sodium carboxymethylcellulose, and sodium sulfate in total.

The MES composition particles of the invention generally have a particle size of ≦ 1.3mm, such as in the range of 0.1 to 1.3 mm. In some embodiments, the MES composition particles of the invention comprise more than 50%, preferably more than 60%, such as 60-70%, 60-65% of the total particles of particles having a particle size of 0.2-0.3 mm. More preferably, in some embodiments, the MES composition particles of the invention comprise more than 75%, such as from 75 to 85%, preferably more than 80%, such as from 80 to 85% of the total particles of particles having a particle size of from 0.2 to 0.5 mm. In a preferred embodiment, more than 90% of the MES composition particles of the invention have a particle size in the range of 0.2 to 0.9 mm. In a more preferred embodiment, more than 97% of the MES composition particles of the invention have a particle size in the range of 0.1 to 0.9 mm.

In a preferred embodiment, the MES composition particles of the invention do not contain zeolites.

The present invention utilizes a fluid bed granulation process to prepare MES composition particles in a fluid bed granulator (also referred to herein as a fluid bed). Compared with extrusion granulation and stirring granulation processes, the method for preparing MES composition particles by adopting the fluidized bed spray granulation process has the advantages of obvious advantages, short operation time, material transfer loss saving among all the working procedures, continuous operation, reduced labor capacity, improved operation conditions, good product quality and capability of preparing MES composition products with good stability and good solubility. More importantly, the fluidized bed granulation process overcomes the defects of large equipment volume, high energy consumption and low energy utilization rate caused by a high tower spraying process for preparing the washing powder, has the advantages of environment-friendly process, small equipment volume, low energy consumption and high energy utilization rate, and accords with the trend of modern social development.

Accordingly, the present invention also provides a process for preparing MES composition particles, comprising:

(1) dissolving a polymer and optionally a sodium silicate in a binder to obtain a liquid containing the polymer, optionally the sodium silicate and the binder;

(2) and (2) contacting a solid mixture containing MES, soda ash, sodium carboxymethylcellulose and sodium sulfate with the liquid containing the polymer, optional sodium silicate and a binder obtained in the step (1) in a fluidized bed, performing fluidized bed granulation, and then drying to obtain MES composition particles.

In the method of the present invention, the solid mixture containing MES, soda ash, sodium carboxymethylcellulose and sodium sulfate (herein referred to simply as solid mixture) contains 20 to 65 parts by mass (e.g., 20 to 60 parts by mass, 30 to 60 parts by mass, 35 to 55 parts by mass) of sodium fatty acid methyl ester sulfonate, 10 to 35 parts by mass (e.g., 10 to 30 parts by mass, 15 to 30 parts by mass, 10 to 25 parts by mass, 15 to 25 parts by mass) of soda ash, 0.05 to 5 parts by mass (e.g., 0.1 to 5 parts by mass, 0.1 to 3 parts by mass, 0.5 to 2.5 parts by mass, 0.5 to 2 parts by mass) of sodium carboxymethylcellulose, and 5 to 65 parts by mass (5 to 60 parts by mass, 5 to 50 parts by mass, 8 to 45 parts by mass, 20 to 45 parts by mass) of sodium sulfate. In certain embodiments, the solid mixture consists of MES, soda ash, sodium carboxymethylcellulose, and sodium sulfate in the above-described parts by mass ratios.

In the process of the invention, the solid mixture is mixed with the liquid containing the polymer, optionally the sodium silicate and the binder in such quantities that: the amount of the polymer used is 0.1 to 10 parts by mass (for example, 0.1 to 7.5 parts by mass, 0.5 to 6 parts by mass, and 0.5 to 5 parts by mass) per 100 parts by mass of the total of the sodium fatty acid methyl ester sulfonate, the soda ash, the sodium carboxymethyl cellulose, and the sodium sulfate, and the amount of the sodium natron used is 0 to 15 parts by mass (for example, 0 to 8 parts by mass, 0 to 5 parts by mass, 0.1 to 8 parts by mass, and 0.1 to 5 parts by mass) per 100 parts by mass of the total of the sodium fatty acid methyl ester sulfonate, the soda ash, the sodium carboxymethyl cellulose, and the sodium sulfate. In some embodiments, the solid mixture is proportioned with the liquid comprising the polymer, optional sodium silicate, and binder in an amount further such that: the amount of the binder is 5 to 75 parts by mass (10 to 75 parts by mass, 20 to 70 parts by mass, 20 to 60 parts by mass, 25 to 60 parts by mass) per 100 parts by mass in total of the sodium fatty acid methyl ester sulfonate, the soda ash, the sodium carboxymethylcellulose, and the sodium sulfate.

The solid mixture is preferably in a fluidized state during granulation. Generally, MES, soda ash, sodium carboxymethylcellulose, and sodium sulfate powder are charged into a fluidized bed, and then air is blown from the bottom of a fluidized bed granulator to mix the powder by air fluidization, thereby obtaining a solid mixture. The temperature of the intake air is usually-10 ℃ to 60 ℃ (for example, 10 ℃ to 50 ℃ or 20 ℃ to 40 ℃), and the relative humidity is usually 20% to 80% (for example, 30% to 60%). Preferably MES, soda ash, sodium carboxymethylcellulose and/or sodium sulfate powder with a particle size of 0.20mm or less, preferably 0.10mm or less, are used for the preparation.

The liquid comprising the polymer, optionally the sodium silicate and the binder is preferably provided in an atomized state. In a preferred embodiment, the liquid containing the polymer, optionally the sodium silicate and the binder is sprayed from top to bottom. When the solid mixture is contacted with a liquid containing the polymer, optional sodium silicate and binder, it is preferred that the solid mixture is in a fluidized state and the liquid containing the polymer, optional sodium silicate and binder is in an atomized state to allow sufficient contact between the two.

In the present invention, the liquid containing the polymer, optionally the sodium silicate and the binder contains the polymer and the binder, optionally also the sodium silicate. In some embodiments, the liquid containing the polymer, optional sodium silicate, and binder consists of the polymer and binder. In other embodiments, the liquid containing the polymer, optional sodium silicate, and binder consists of the polymer, sodium silicate, and binder.

In some embodiments, the liquid containing the polymer, optional sodium silicate, and binder comprises 0.1 to 10 parts by mass (e.g., 0.1 to 7.5 parts by mass, 0.5 to 6 parts by mass, 0.5 to 5 parts by mass) of the polymer, 0 to 15 parts by mass (e.g., 0 to 8 parts by mass, 0 to 5 parts by mass, 0.1 to 8 parts by mass, 0.1 to 5 parts by mass) of sodium silicate, and 5 to 75 parts by mass (10 to 75 parts by mass, 20 to 70 parts by mass, 20 to 60 parts by mass, 25 to 60 parts by mass) of the binder.

The adhesive suitable for the present invention includes but is not limited to one or a combination of more than one of water, alcohol, propylene glycol and glycerin.

In some embodiments, the binder is water, or consists of water and one or more solvents selected from the group consisting of alcohol, propylene glycol, and glycerin. In embodiments where the binder contains water, the amount of water in the binder is not particularly limited, for example, the amount of water may be from 10% to 90% by weight of the total weight of the binder, such as from 1/3 to 2/3. In certain embodiments, the binder is a mixture of water and glycerin; preferably, the mass ratio of water to glycerol is 1/3-2/3, such as 2/3. In certain embodiments, the binder is a mixture of water and ethanol; preferably, the mass ratio of the water to the ethanol is 1/3-2/3, such as 1/2 and 1/3.

Generally, the mass ratio between the adhesive and the solid mixture is 0.1-1.5: 2, for example 0.2 to 1.5: 2. 0.4-1.4: 2. 0.4-1.2: 2. 0.5-1.2: 2, the amount of the binder may be 5 to 75 parts by mass, for example, 10 to 75 parts by mass, 20 to 70 parts by mass, 20 to 60 parts by mass, 25 to 60 parts by mass, based on 100 parts by mass of the total amount of MES, soda ash, sodium carboxymethylcellulose and sodium sulfate.

After the granulation, the granules obtained by the granulation were dried to obtain MES composition granules of the present invention. The drying temperature can be the drying temperature conventional in the art, such as 20-70 ℃ and 30-65 ℃. Drying may be carried out in a fluidised bed.

In certain embodiments, drying further comprises a sieving step, wherein the particles remaining on the sieve are MES composition particles of the present invention. In certain embodiments, the mesh size of the screen is 150 mesh.

The fluidized bed granulator used for preparing MES composition particles comprises a fluidized bed body, a gas distribution device, a gas pipeline for the fluidized bed, a heater, a spraying device and a dust removal device.

The process for preparing MES composition particles of the present invention is schematically described below in connection with fig. 1. The air discharging and inlet of the fluidized bed main body 1 are carried out by a blower 7, an air filter 8 is arranged at an air inlet and used for purifying air, and the purified air enters the fluidized bed from the bottom of the fluidized bed through a gas distribution plate after being heated to a certain temperature in a heater 9. Under the action of hot air, the powder on the bed layer is fluidized and contacted with atomized liquid containing polymer, optional sodium silicate and adhesive sprayed from nozzle in the central part of fluidized bed, so that the liquid forms bridges between powder and is coagulated and grown into particles. The powder not contacted with the adhesive is collected by a dust recovery device, and the air is discharged out of the equipment after being filtered. And after granulation is finished, stopping spraying, increasing the air inlet temperature of hot air, starting drying, sieving after drying is finished, returning the fine powder to the fluidized bed for granulation again, and obtaining MES composition particles on the sieve.

Generally, 20-65 parts by mass of MES, 10-35 parts by mass of soda ash, 0.05-5 parts by mass of sodium carboxymethylcellulose and 5-65 parts by mass of sodium sulfate are crushed and sieved to form fine powder with the particle size of less than or equal to 0.20mm, preferably less than or equal to 0.10mm, the fine powder is put into a closed fluidized bed, air is introduced from the bottom of the fluidized bed, fluidization is carried out by air, and powder mixing is carried out to obtain a solid mixture; dissolving 0.1-10 parts by mass of polymer and 0-15 parts by mass of sodium silicate in 5-75 parts by mass of a binder to prepare a liquid containing the polymer, optional sodium silicate and the binder, spraying the atomized liquid containing the polymer, optional sodium silicate and the binder from top to bottom in a fluidized bed, fully contacting with a fluidized solid mixture for fluidized bed granulation, drying in the fluidized bed after the granulation is finished, sieving by a sieve of 150 meshes to obtain final MES composition particles, and collecting the solid mixture which does not form the MES composition particles and returning the solid mixture to the fluidized bed for re-granulation. The mass ratio of the adhesive to the solid mixture is 0.1-1.5: 2. the air inlet temperature at the bottom of the fluidized bed is-10-60 ℃, the relative humidity is 20-80% and the drying temperature is 20-70 ℃ during granulation.

The invention also provides the application of the MES composition particles in the preparation of detergents, especially washing powder, or in washing. The washing may be various types of washing, such as washing applied to laundry powder.

The MES composition particles of the invention have MES content of over 60 wt%. The MES composition particles can be used as a post ingredient to be added into a detergent such as washing powder, or used as a base powder (a pre ingredient) to be compounded and then prepared into the detergent such as the washing powder, or directly used as the detergent, and can prepare a detergent product with high MES content and good performance. The MES composition particles are used in the detergent, the problem of application of natural and renewable raw material MES in the detergent is solved, and the detergent has strong detergency, high bulk density, good solubility, good fluidity, less fine powder, pressure resistance, difficult breakage and difficult caking.

The MES composition particles of the invention may be used as a postdose or base powder to prepare detergents, especially laundry detergents, by methods conventional in the art. For example, the MES composition particles may be prepared as a postdose or as a base powder by simple mixing with other components of a laundry powder.

The invention also provides a detergent, in particular a washing powder, comprising MES composition particles according to the invention.

Other ingredients in detergents, such as laundry powders, are well known in the art and include, but are not limited to, any one or more of fatty alcohol-polyoxyethylene ether (AEO-9), soda ash, sodium silicate, active enzymes, polymers, sodium carboxymethylcellulose (CMC), optical brighteners, perfumes, and anhydrous sodium sulphate. These ingredients are also used in amounts conventional in the art.

Compared with the prior art, the invention has the following advantages:

(1) MES composition particles have stable performance in the production process, and MES is not easy to hydrolyze;

(2) MES composition particles have good solubility at room temperature and also good solubility at low temperatures (10 ℃);

(3) the MES composition particles do not contain zeolite, are stable during storage, have good particle fluidity, are not choked, are not easy to agglomerate and are not easy to break;

(4) the MES composition particles have MES content over 60%, and may be used as base powder, post-compounding material, washing powder, etc. to prepare washing powder product with high MES content and high performance.

The present invention will be described in detail with reference to examples, but the present invention is not limited thereto. The experimental procedures used in the following examples are, unless otherwise specified, conventional procedures or procedures recommended by the reference manufacturers. The materials, reagents, apparatuses and the like used in the following examples are, unless otherwise specified, those conventional in the art and can be obtained from public sources. In the description of the present invention and the following examples, "%" represents weight percent, "parts" represents parts by weight, and proportions represent weight ratios, unless otherwise specified.

The MES starting material used in the following examples is a commercial MES powder having an active content of 87% to 92% (C16 FR).

The product performance test methods referred to in the following test examples are illustrated below:

(1) fluidity: referring to the measurement of GBT 11986 surfactant powder and particle angle of repose, a special funnel is fixed at a certain height above a horizontal plate, a powder or granular sample of a given volume is passed through the funnel, and the angle of repose of the obtained cone is determined, the smaller the angle of repose, the better the fluidity of the sample.

(2) Room temperature solubility (% insoluble content): dissolving 1g sample in 250g of 250ppm hard water at room temperature of 25 ℃, stirring at 250rpm for 1min, filtering by using rapid qualitative filter paper, filtering by using constant weight filter paper, calculating the weight of the residue, and subtracting the content of zeolite in the sample (the zeolite is not dissolved and remains on the filter paper) if the zeolite exists in the sample to obtain the content of insoluble substances. According to the solubility test method, the insoluble content of common washing powder is less than 2% (no zeolite is contained).

(3) Low temperature solubility (% insoluble content): dissolving 0.5g sample in 500g of 250ppm hard water at 10 deg.C, stirring at 250rpm for 5min, filtering with rapid qualitative filter paper, filtering with constant weight filter paper, calculating the weight of the residue, and subtracting the zeolite content (insoluble zeolite, residual zeolite on filter paper) if zeolite exists in the sample to obtain the insoluble substance content.

(4) Anti-caking property: installing an anti-caking performance tester (model: CJLY-5-67.5, Albee company, Alby, USA), placing a gasket at the bottom of a container at the lower part of the anti-caking performance tester, sleeving a cylinder, and tightly hooping the cylinder by using a hoop; pouring the tested washing powder into a container at the lower part of the anti-caking performance tester until the washing powder overflows, and leveling the upper surface of the washing powder by using a ruler; placing a gasket on the surface of the powder, loosening the pin, slightly putting down the pressure rod, and allowing the pressure rod to flexibly fall down to enable the lower disc to be just pressed on the gasket; adding two 5KG weights on the compression bar disc, maintaining for 2 minutes, and then taking down the weights; taking down the weight of 5KG, lifting the pressure lever, inserting the pin, carefully detaching the clamp, and removing the container; adding weights on the gasket: firstly, estimating an initial value, adding a corresponding weight, keeping for 10s, then adding the weight until most of the powder falls off and collapses, and recording the total weight of the added weight. The smaller the weight, the better the anti-caking performance of the washing powder, and the larger the weight, the worse the anti-caking performance of the washing powder.

(5) Detergency performance: according to the requirements of concentrated powder WL-B in national standard of GBT 13171.2-2009 laundry powder, the sample is respectively used for measuring the decontamination ratios of J-01, J-02 and J-03 polluted cloth according to the concentration of 0.1%, and the larger the ratio is, the better the decontamination performance is.

(6) Active content and disodium salt content: the active matter content determination method refers to the national standard: GB/T13173-2008 surfactant detergent test method, disodium salt content determination method reference row mark: QBT4081-2010 sodium fatty acid methyl ester sulfonate. Actives are defined herein as in GB/T13173-2008 surfactant detergent test method and disodium salt is defined as in QBT4081-2010 sodium methyl fatty acid ester sulfonate.