CN114149867B

CN114149867B - Solid fabric softening composition

Info

Publication number: CN114149867B
Application number: CN202111296894.XA
Authority: CN
Inventors: 林焕容; 邱振名; 张利萍; 周文杰; 黄亮
Original assignee: Guangzhou Liby Enterprise Group Co Ltd
Current assignee: Guangzhou Liby Enterprise Group Co Ltd
Priority date: 2021-11-03
Filing date: 2021-11-03
Publication date: 2023-11-24
Anticipated expiration: 2041-11-03
Also published as: CN114149867A

Abstract

The invention discloses a solid fabric softening composition, which comprises the following components: 40-95% of polyethylene glycol, 0.5-5% of cationic polymer, 0.01-5% of fragrance stabilizing auxiliary agent, 0.1-5% of forming auxiliary agent, 0.1-15% of spice and 0.01-30% of other auxiliary agents. The side chain of the cationic polymer contains polyoxyethylene groups, and the average ethoxylation degree is 1-20. The composition particles provided by the invention are close to the shape of ideal size, and are co-stored with the fabric and the detergent in the main washing stage and after rinsing, the fabric has obvious perceivable softening effect, meanwhile, the detergency of the detergent is not reduced, the compatibility of solid particles and the polyvinyl alcohol water-soluble film can be improved, and the stability of odor between the polyethylene glycol PEG perfuming particle composition and the water-soluble film is obviously improved.

Description

Solid fabric softening composition

Technical Field

The invention relates to the technical field of detergents, in particular to a solid fabric softening composition which contains a fragrance stabilizing auxiliary agent and a forming auxiliary agent and does not cause the reduction of detergency.

Background

In daily washing of fabrics, the washing and softening products are added according to recommended amounts in a washing time stage in order to achieve better cleaning and softening effects. For convenience, the user typically puts the detergent and softener into the washing machine at the same time, and this method does not provide the desired cleaning and softening effect for the fabric, because the detergent typically contains an anionic surfactant to clean the laundry, and the softener typically contains a cationic surfactant to soften the fabric, and if both are simultaneously mixed for the main wash stage, the anionic and cationic surfactants precipitate due to the action of charges and cannot exert their respective effects, and the cleaning performance and softening effect are reduced.

The solid particles using polyethylene glycol (PEG) as water-soluble carrier, the shaping and dissolving time of the product particles are affected by the molecular weight of PEG to a certain extent, and the viscosity of slurry and the cooling shaping of the particles during granulation are affected by the different viscosity and melting point of PEG with different molecular weights. The formability of the solid particles is not only influenced by the molecular weight of polyethylene glycol, but also by other components, such as the addition of perfume, other auxiliary agents, surfactants and the like, which enable the prepared slurry to be thinner or change the surface property of the slurry, so that the contact angle of the slurry falling onto a cooling steel belt after demolding becomes larger, the solidified particles collapse, and the full and soft aesthetic feeling of the product is influenced.

Consumers have increasingly higher requirements on the fragrance of washing products, and hope that washed clothes can have lasting pleasant fragrance, when the fragrance is used as a content to be wrapped in a polyvinyl alcohol (PVA) water-soluble film to form solid particle coagulated beads, the compatibility problem of the content and the PVA film can occur, for example, after the washing products are placed for a period of time, the solid particle coagulated beads generate unpleasant smell to bring bad use experience to consumers, and the washing products belong to the quality problem that the products cannot be ignored.

Chinese patent CN 111655831A discloses a particulate laundry softening detergent additive which can be used with laundry detergents and provides softening of the whole wash during the washing step, but does not address the problem of negative impact on soil release due to the co-presence of softening additive and laundry detergent in the main wash stage. Chinese patent CN 104854229B discloses a laundry fragrance additive, 2000 to 13000 molecular weight polyethylene glycol as a main component, by the addition of a balancing agent to produce particles of desired size and shape, but does not relate to a method how to adjust the particle formability by a balancing agent. Chinese patent CN 110607208A discloses particulate laundry detergent compositions comprising perfume particles and methods of use thereof, the aspect ratio of the perfume particles being specified, but does not describe how to adjust or achieve this ratio. Chinese patent CN111286414 a discloses a specific nonionic surfactant or nonionic modified polyethylene glycol to facilitate the molding of the beads and solve the technical problem that the surfactant cannot be added to the polyethylene glycol carrier, but does not relate to how to adjust and improve the molding of the bead base slurry. With the rapid development of the product with outstanding portability, when the solid perfuming particles are wrapped in the polyvinyl alcohol water-soluble film, the solid perfuming particles and the polyvinyl alcohol water-soluble film are interacted with the PVA film after being placed in a constant temperature and humidity environment for a period of time due to higher essence content, so that some unpleasant odors usually appear, and the compatibility of the solid perfuming particles and the polyvinyl alcohol water-soluble film is improved, and the stability of the product in shelf life is also an urgent problem to be solved.

Disclosure of Invention

Aiming at the problem that the detergent and the softener are mutually influenced when the detergent and the softener are simultaneously present in a main washing stage in the prior art, the invention provides the solid fabric softening composition which has a softening effect and does not cause the reduction of the detergency of the detergent, and simultaneously, the problems of compatibility of solid perfuming particles and a polyvinyl alcohol water-soluble film, stability of the odor shelf life of a product and the plumpness of the product particles are solved.

The invention provides a solid fabric softening composition comprising the following components: 40-95% of polyethylene glycol, 0.5-5% of cationic polymer, 0.01-5% of fragrance stabilizing auxiliary agent, 0.1-5% of forming auxiliary agent, 0.1-15% of spice and 0.01-30% of other auxiliary agents. The polyethylene glycol has a molecular weight in the range of 2000 to 10000, preferably 4000 to 8000. The cationic polymer has a weight average molecular weight ranging from 50000 to 2000000, preferably from 100000 to 1000000, and a polyoxyethylene group in the side chain, the average degree of ethoxylation being from 1 to 20.

The forming aid is selected from one or more mixtures of fatty alcohols, preferably C8-C22 fatty alcohols, more preferably one or more mixtures of C14-C18 fatty alcohols.

The cationic POLYMER is selected from the group consisting of cellulose POLYMERs containing quaternary ammonium groups, cationic guar gum derivatives, chitosan and its derivatives, polyethylenimine and its derivatives, preferably cationic POLYMERs provided in solid powder form or in anhydrous state, such as POTYQUTA 400 and POTYQUTA 400LR from Tianci company, SOFTCAT SX-400X from Dow company, SUPRACARE 133POLYMER, and the like.

The cationic polymer may have a charge density of about 0.05 to 15meq/g (meq is milliequivalent), preferably about 0.1 to 10meq/g, more preferably 0.1 to 2meq/g.

Polyethylene glycol suitable for the present invention may be selected from commercial products such as CARBOWAX Polyethylene Glycol from Dow, PLURIOL E8000 from Basf, polyKOL 8000S from Clariant.

The fragrance stabilizing auxiliary is selected from at least one of common chelating agents such as amino carboxylic acids and organic phosphonic acids. In PEG solid particle products with high essence content packaged by PVA film, the inventor finds that the chelating agent can effectively relieve the effects of essence and PVA film, the generated sour taste and the peculiar smell generated by the change of the essence. Preferably, the aminocarboxylic acid is one or more of ethylenediamine tetraacetic acid (EDTA) salt, aminotriacetic acid (NTA) salt, ethylenediamine tetramethylene phosphoric acid (EDTMP) salt of organic phosphonic acid type, aminotrimethylene phosphoric Acid (ATMP) salt, diethylenetriamine pentamethylene phosphonic acid (DTPMP) salt, hydroxyethylidene diphosphate (HEDP) salt.

The perfume comprises a commercially available liquid perfume and a microcapsule perfume which can be freely selected to be suitable for the consumer group of the product. The liquid fragrance preferably has a flash point above 75 ℃. The microcapsule perfume is a micro-container made of natural or synthetic polymer materials, and the droplet perfume is completely encapsulated in the micro-container to form the microcapsule perfume, the size of the microcapsule perfume is 1-100 mu m, and the fragrance retaining effect of the fabric is maintained. The microcapsule particles are insoluble in water in the washing process and are easy to deposit on clothes, and after the clothes are dried, the microcapsule particles are broken along with friction in the wearing process to release the encapsulated perfume, so that the purpose of keeping fragrance for a long time is achieved. The microcapsule perfume suitable for the invention can be selected from microcapsule perfumes wrapped by chitosan or modified derivatives thereof, polyurethane, melamine formaldehyde resin, urea formaldehyde resin, acacia-maltodextrin, starch-maltodextrin and other materials, and can be added with cationic monomers for positive charge modification so as to achieve better deposition effect. The microencapsulated fragrance suitable for the present invention may be selected from commercial goods such as from the company Fenmeiyi, qi Hua Du, dexin, international perfumery or other suitable sources.

Other auxiliary agents, such as one or more than two of cationic surfactant, organosilicon polymer, colorant, antioxidant, ultraviolet inhibitor, antibacterial agent, long-acting antibacterial agent, anti-cross dye agent and other water-soluble carriers except polyethylene glycol PEG, are added according to product appearance color, functional requirements, cost control and the like.

Drawings

Fig. 1 is a schematic diagram of particles of an example.

Detailed Description

All percentages, fractions and ratios are by weight of the total composition of the present invention, unless otherwise specified. All molecular weights are weight average molecular weights as expressed in daltons, with respect to the amount of active agent given by all weights of ingredients listed, unless indicated otherwise.

The solid fabric softening composition provided by the invention can be put into a washing machine cylinder together with fabrics and coexist with a detergent in a main washing stage. The solid fabric softening compositions of the present invention include, but are not limited to, a plurality of solid particles dosed in a metered dose requiring a measuring cup, and also include solid gel bead forms encapsulated with a polyvinyl alcohol water soluble film.

Solid fabric softening compositions typically comprise a polyethylene glycol PEG water soluble carrier, a cationic polymer, and may also comprise fragrance stabilizing aids, forming aids, perfumes, other aids and the like.

The solid fabric softening composition described above, wherein the total moisture content of the individual components of the plurality of particles is less than 5% by weight, is preferably provided in an anhydrous state.

The polyethylene glycol according to the invention is present in the solid softening composition in an amount of 40 to 95% by weight, preferably 50 to 85% by weight.

The cationic polymer of the present invention is present in the solid softening composition in an amount of from 0.5% to 5%, preferably from 1% to 3% by weight, and provides effective softening to the fabric when used alone or in combination with a fabric softening aid.

The fragrance stabilizing aid in the present invention is a chelating agent in an amount of 0.01 to 5%, preferably 0.1 to 2%, more preferably 0.15 to 0.5% by mass of the solid softening composition.

The chelating agent is selected from at least one of amino carboxylic acids and organic phosphonic acids. Preferably, one or more of ethylenediamine tetramethylene phosphate (EDTMP) salt, aminotrimethylene phosphate (ATMP) salt, diethylenetriamine pentamethylene phosphate (DTPMP) salt, hydroxyethylidene diphosphate (HEDP) salt. The chelating agent can remarkably improve the compatibility of the content and the polyvinyl alcohol PVA water-soluble film, and particularly obviously slow down unpleasant odor generated by the content and the polyvinyl alcohol PVA water-soluble film after being placed for a period of time or stored under heat.

The forming aids of the present invention are present in the solid softening composition in an amount of from 0.1 to 5% by weight, preferably from 0.5 to 3.5% by weight. The forming auxiliary agent is selected from C8-C22 fatty alcohol, more preferably C14-C18 fatty alcohol, and can be one or more than two of C14 fatty alcohol, C16 fatty alcohol and C18 fatty alcohol.

The perfume in the present invention comprises at least one of unencapsulated liquid perfume and microencapsulated perfume in an amount of from 0.1 to 15%, preferably from 3 to 10% by weight of the solid softening composition.

The liquid perfume can be freely selected from commercial liquid perfumes suitable for consumer groups of the product, and preferably has a flash point of above 75 ℃.

The microcapsule perfume is a micro-container made of natural or synthetic polymer materials, and the droplet perfume is completely encapsulated in the micro-container to form the microcapsule perfume, the size of the microcapsule perfume is 1-100 mu m, and the fragrance retaining effect of the fabric is maintained. The microcapsule particles are insoluble in water in the washing process and are easy to deposit on clothes, and when the clothes are dried, the microcapsule particles are broken along with friction in the wearing process to release the wrapped perfume, so that the purpose of keeping fragrance for a long time is achieved. The microcapsule perfume suitable for the invention can be selected from microcapsule perfumes wrapped by chitosan or modified derivatives thereof, polyurethane, melamine formaldehyde resin, urea formaldehyde resin, acacia-maltodextrin, starch-maltodextrin and other materials, and can be added with cationic monomers for positive charge modification so as to achieve better deposition effect. The microencapsulated fragrance suitable for the present invention may be selected from commercial goods such as from the company Fenmeiyi, qi Hua Du, dexin, international perfumery or other suitable sources.

The weight percentage of other auxiliary agents in the solid soft composition is 0.01-30%. According to the product appearance color, functional requirement, cost control, etc., one or more of cationic surfactant, organosilicon polymer, colorant, antioxidant, ultraviolet inhibitor, long-acting antibacterial agent, anti-cross dye agent, and other hydrotropic agent except polyethylene glycol PEG can be optionally added.

Softening aids such as cationic surfactants and/or silicone polymers may be included in the solid softening composition which when used with cationic polymers act synergistically to soften fabrics, the weight percentage of the solid softening composition being from 0.1 to 20%, preferably from 3 to 15%.

The cationic surfactant is one or more selected from esterquat, amidyl quat, imidazoline quat and alkyl quat, preferably esterquat with good biodegradability.

The silicone is selected from one or more than two of silicone polyether, amino silicone, cationic silicone, ethoxylated silicone, propoxylated silicone, and polydimethylsiloxane, preferably cationic silicone, amino silicone, polyether modified amino silicone oil, and polydimethylsiloxane, wherein the polydimethylsiloxane preferably has a viscosity of between 6,000cSt and 1,000,000 cSt.

The solid fabric softening composition may comprise an antioxidant to enhance the stability of the colour and/or odour of the solid particles during the shelf life of the product, to provide a product of stable quality throughout the life of the product, the weight percentage content in the solid fabric softening composition being from 0.001 to 1%, preferably from 0.01 to 0.2%. The antioxidant can be butylated hydroxytoluene, dibutylhydroxytoluene (BHT), butylated Hydroxyanisole (BHA), sodium metabisulfite used in daily chemical industry.

The solid fabric softening composition may comprise an anti-uv agent to reduce the effect of the solid particles from uv light on the appearance and/or odour of the product during manufacture, storage, use etc. the weight percentage of the solid fabric softening composition is from 0.001 to 1%, preferably from 0.01 to 0.2%. Suitable anti-uv agents may be benzophenones, benzotriazoles, salicylates, substituted acrylonitriles.

The solid fabric softening composition can contain a long-acting antibacterial agent, has a long-acting antibacterial effect on the treated fabric, meets the requirements of partial consumers, and has a weight percentage of 0.1-1%. The long-acting antibacterial agent can be benzalkonium chloride, hydroxy dichloro diphenyl ether, nano silver solution and parachlorometaxylenol.

The solid fabric softening composition may comprise a stain blocker which is effective to inhibit the cross-staining of fabrics caused by the transfer of dye or dyes to each other on the fabrics during the wash process, the weight percentage of said solid fabric softening composition being in the range of from 0.01% to 3%, preferably from 0.1% to 1.0%. Suitable anti-cross-linking agents, such as polyamine N-oxide polymers, copolymers of N-vinylpyrrolidone and N-vinylimidazole, polyvinylpyrrolidone polymers, ethoxylated polyethyleneimines.

Besides PEG, other water-soluble carriers, i.e. disintegrants, are effective in regulating the dissolution time of the solid composition at the stage of use, and suitable dissolution time is advantageous in reducing the residue of solid particles after washing is completed, the weight percentage content in the solid soft composition being 1-20%, preferably 3-10%. The disintegrating agent is one or more selected from monosaccharide, disaccharide, polysaccharide, carbonate, sulfate, citrate, lactate, silicate, sorbate, sodium salt, potassium salt, and starch, preferably monosaccharide, disaccharide, and polysaccharide.

The particles referred to in the present invention are selected from the following shapes: cylindrical, conical, circular, oval, hemispherical, spherical, flat hemispherical, and combinations thereof, preferably hemispherical or flat hemispherical in shape. Flat hemispherical refers to a shape in which the particle portion is flattened so that the average curved curvature is smaller than the hemispherical curvature having the same radius. The moldability test of the solid particles in the present invention is carried out by taking a hemispherical shape or a compressed hemispherical shape as an example, a ratio of a highest height of the bottom to a radius of the bottom orthogonal to not less than 0.5, more preferably between 0.6 and 1.0.

The particles have a single mass of about 10mg to 1500mg, preferably a single mass of about 10mg to 200mg, more preferably a single mass of about 30mg to 150mg, or a combination thereof. The maximum particle size is between 1mm and 20mm, preferably between 3mm and 10mm, or a combination of the above. Theoretically, the size of the particles is proportional to the dissolution time, i.e. the larger the particles the slower the dissolution time in water.

The time from the dispersion of the particles in pure water at 25 ℃ to the visual observation of no visible particles as the dispersion in water is measured, and the dissolution time of the particles is about 7 minutes to 30 minutes, preferably about 8 minutes to 20 minutes, more preferably about 8 to 15 minutes.

Test and criteria for embodiments

1. Stability test method

High temperature stability: after the composition is bottled and sealed, the composition is placed at a temperature of 45+/-2 ℃ for 4 weeks at constant temperature, and the appearance and the smell are observed under the environment of room temperature of 25+/-5 ℃.

Low temperature stability: after the composition is bottled and sealed, the composition is placed at a constant temperature of 0+/-2 ℃ for 4 weeks, and the appearance and the smell are observed in an environment of 25+/-5 ℃ at room temperature.

Stability at normal temperature: the composition is bottled and sealed, and then placed at 25+/-5 ℃ for 4 weeks, and is directly observed.

High temperature and high humidity stability: the composition is wrapped in a polyvinyl alcohol PVA water-soluble film, bottled and sealed, placed at 45+/-2 ℃ and 70% RH, kept at constant temperature for 4 weeks, and restored to room temperature at 25+/-5 ℃ for observing the appearance and smell.

2. Stability evaluation criterion

The "-" indicates that the sample has no obvious change in smell and appearance, belongs to an acceptable range and has qualified stability;

the samples were severe in appearance discoloration or produced unpleasant odors, failed in stability, and the number of "+" indicated the severity of discoloration and off-flavors, the more pronounced the anomaly, the more unstable the sample.

3. Method for testing influence on detergency

The detergency of the invention refers to the capability of a fabric detergent to remove different stains, and a common cationic polymer and cationic surfactant with softening effect can have negative influence on the cleaning capability of the detergent, and the detergent and the softening composition are added into a vertical type decontamination machine according to the recommended use concentration for national standard washing. The test is carried out according to the method of the national standard GB/T13174-2008. The whiteness W1 of the three kinds of dirty cloth before washing is measured by adopting national standard carbon black, protein and sebum three kinds of dirty cloth and a WSD-3U fluorescent whiteness meter. Hard water with the hardness of 250ppm is prepared according to the GB/T13174-2008 standard, the RHLQ type vertical detergent is adopted to finish one-time washing, the addition amount of the detergent is 2g/L, the concentration is 0.7g/L, and the soft composition is added according to the recommended use concentration. The washing time is 20min, the washing temperature is 30 ℃, the stirring speed is 120r/min, the washed dirty cloth is rinsed, dried, the whiteness W2 of the washed cloth piece is tested by a whiteness meter, and the whiteness difference DeltaW is calculated as follows:

Δw=w2-W1; wherein W2 is whiteness after washing, and W1 is whiteness before washing.

The detergency of the test sample is compared with the detergency of the national standard detergent to calculate a P value,

p= Δw sample/- Δw standard; the delta W sample is the whiteness difference of the dirty cloth before and after washing by the sample detergent, and the delta W standard is the whiteness difference of the dirty cloth before and after washing by the national standard detergent.

Test detergent + softening composition or liquid softener when washing simultaneously, the relative ratio of decontamination when using the detergent alone is compared and calculated to obtain delta P value,

△P _i ＝P ₀ -P _n the method comprises the steps of carrying out a first treatment on the surface of the Wherein P is ₀ For the detergency ratio of detergents, P _n For the soil release ratio of the detergent + softening composition or liquid softener with washing, i is the sample tested or the combined sample.

E _i ＝∑(△P _i )/n；E _i The average value of the decontamination ratio of the detergent plus the softening combination or the liquid softener during the simultaneous washing is given, and n is the number of the tested stained cloths.

4. Evaluation criteria for influence on detergency

The impact criteria for a softening composition on detergent cleaning power using the E value are as follows:

TABLE 1 detergency impact evaluation criteria

Average decontamination ratio difference E _i	Description of the invention	Evaluation rating of detergency impact
			Greater than 0.5	Has great influence on decontamination	+++
0.5—0.2	Has great influence on decontamination	++
			0.2—0.05	Has no influence on decontamination	+
＜0.05	Has no influence on decontamination	±

When the detergency-impact evaluation scale is +or.+ -., it is generally considered that the softening composition does not decrease the detergency of the detergent or does not significantly decrease, i.e., it is judged that there is no impact on detergency.

5. Soft evaluation test method

According to the softness evaluation test method, the daily use mode of a consumer is completely simulated, and the softness effect is evaluated after the fabrics of different fabrics are washed. The newly purchased fabric was subjected to alkali treatment and high temperature treatment several times in order to obtain a coarse dry test fabric. The total washing test method of the Siemens drum washing machine is adopted, the mixed mode is adopted, the single cycle washing time is 45 minutes (including primary rinsing and 2 rinsing), the water hardness is about 130ppm, and the washing temperature is 25 ℃. The total fabric load weight was about 3kg, including half weight of pure cotton towel and half weight of polyester cotton blend fabric. The test sample and the detergent are simultaneously put into the main washing stage, and the liquid softener is added during the secondary rinsing. 30 volunteers, who were habituated to using liquid softener at ordinary times, were selected and the washed dry towels were scored for softness.

6. Softness evaluation criterion

Softness evaluation criteria are as follows.

TABLE 2 softness evaluation criteria

Test sample	Washing with detergent only (blank)	Adding softener for secondary rinsing
			Score value	0 point	5 minutes

For scoring of the softness evaluation samples, the score may be higher than 5 or lower than 0, the higher the softness, the higher the score.

7. Method for evaluating particle formability

The particle formability of the present invention is evaluated using a hemispherical shape, a flat hemispherical shape, as shown in fig. 1, but is not limited to these two shapes. The radius d of the particle is the distance from the curved surface point A to the sphere center 0, the distance from the sphere center O to the highest point C of the curved surface is the hemispherical height r, and when the ratio q of r to d is closer to 1.0, the obtained particle is closer to the hemispherical shape.

8. Evaluation criterion for particle formability

The evaluation criteria for particle formability, based on the particle size and the individual mass being in the proper range, require a particle size between 3mm and 10mm, an individual gram weight between 30mg and 100mg, are evaluated mainly from the ratio q of the particle heights r and d, as follows:

TABLE 3 formability evaluation criteria Table

When the ratio q is between 0.8 and 1.0, the particles are more similar to or in the shape of a hemisphere, the particle size is full, the appearance is more aesthetically significant, and the shape sought by the particles of the solid fabric composition is also the shape sought by the particles of the solid fabric composition.

9. Odor assessment method

The odor evaluation method in the present invention means that when the solid soft composition is wrapped in a polyvinyl alcohol PVA water-soluble film, it is placed in a sales package in an environment of 45 ℃ and 70% rh for 4 weeks, and then taken out and recovered to room temperature (25 ℃) and compared with a sample placed in an environment of normal temperature (25 ℃) for 4 weeks. 30 volunteers, preferably those sensitive to smell, were selected and the smell after opening or uncovering the bag for the heat-stored and normal temperature samples was evaluated by sensory evaluation.

10. Odor evaluation criteria

Volunteers evaluate the flavor and intensity between the heat storage sample and the normal temperature sample, the closer the two are, the higher the score is, and when the volunteers judge that the samples are completely consistent and no unpleasant odor (peculiar smell) is generated, the score is 5; when the two are judged to be different and have unpleasant odor, the score is 0; the score is between 0 and 5, the graduation value is 0.5, the higher the score is, the higher the acceptability is, in other words, the higher the score is, the better the odor stability of the sample is, and the average score calculation formula of the odor stability of the test sample is as follows:

R _i ＝∑(A _i )/n

wherein:

i-the i-th test sample;

A _i -score of the ith test sample;

n—number of participating test consumers, n=30.

11. Methods of formulation and use

The solid fabric softening compositions of the present invention are prepared by various methods well known to those skilled in the art. The formulation of the composition may be carried out by conventional means, with the appropriate processing temperature and processing time being chosen based on the state and effect of the components in the PEG melt, as well as the stability of the components. The method comprises the following steps:

(1) Adding polyethylene glycol into a stirring pot, heating to 85deg.C until the polyethylene glycol is transparent liquid, or melting polyethylene glycol in a drying room, and adding into the stirring pot.

(2) Adding the cationic polymer, the forming auxiliary agent and the fragrance stabilizing auxiliary agent into a stirring pot, stirring and dispersing uniformly, and starting a cooling procedure to ensure that the temperature of the stirring pot is kept at 70 ℃.

(3) Adding perfume and other auxiliary agents, stirring and mixing uniformly, conveying to a liquid-solid conversion granulator, and cooling by a steel belt to obtain soft fabric particles.

The methods of using the solid fabric softener compositions of the invention are well known to those skilled in the art, as are typical methods of use such as fragrance retaining beads, the softening compositions are manually dosed in a measuring cup or packaged in a dosed manner on a polyvinyl alcohol PVA water-soluble film, the softening compositions are dosed into a washing machine together with fabric, detergent, and are brought into coexistence with the detergent and contact with the surface of the article to be washed, and the machine washing comprises a full wash process such as a main wash step, a rinse step, etc.

Without further elaboration, it is believed that one skilled in the art can, using the preceding description, utilize the present invention to its fullest extent. The following examples are intended to further illustrate and demonstrate embodiments within the scope of the present invention. Thus, the examples are to be understood as merely illustrative of the invention in more detail, in which, unless otherwise indicated, all amounts are by weight and the amounts of the ingredients listed are amounts of the active substances in conversion.

In the examples below, the following abbreviations will be used and have the indicated functions.

PEG8000: polyethylene glycol 8000, water-soluble carrier.

Cationic polymer: cellulose polymers containing quaternary ammonium groups, fabric softeners.

EDTA-2Na: ethylenediamine tetraacetic acid-disodium, fragrance stabilizing aid.

EDTA-4Na: ethylenediamine tetraacetic acid-tetrasodium salt, a fragrance stabilizing aid.

EDTMPS, ethylenediamine tetramethylene sodium phosphate, fragrance stabilizing additive.

HEDP-2Na, hydroxy ethylidene diphosphonic acid-disodium, fragrance stabilizing additive.

HEDP-4Na: hydroxy ethylidene diphosphonic acid-tetrasodium, a fragrance stabilizing aid.

Fatty alcohol: C14-C18 fatty alcohols, forming aids.

Organic silicone oil: one of amino silicone oil, polyether modified amino silicone oil and polydimethylsiloxane, and a fabric softening auxiliary agent.

Specific data of the examples

1. Softness assessment test

Comparative example 1 is a commercially available compliant bead, comparative example 1 is a solid particle of PEG carrier, and a single use of between 20 grams and 40 grams is recommended, with an add-on of 20 grams for this test.

Comparative example 2 is a commercially available liquid softener, the cationic surfactant is about 4%, a single use of between 40 grams and 80 grams is recommended, the test addition is 40 grams, and the use case of comparative example 2 of table 4 is that of a fabric and a detergent at the same time.

Examples 1, 2 and 3, the present example used the prior art technique with polyethylene glycol as the water-soluble carrier, the formulation procedure was as described, the components and amounts are as shown in table 4, the test single dose was 8 grams, as follows:

TABLE 4 composition and softening score of solid fabric softening compositions of examples 1, 2, 3

As can be seen from the average softening scores in Table 4, the solid softening composition of the present invention can achieve a more desirable softening effect when used in an amount of 2/5 of comparative example 1 and 1/5 of comparative example 2.

2. Detergency impact test

Evaluation of detergency effect comparative example 2 will co-exist with fabrics, detergent during the full wash of both main wash and rinse phases.

The solid fabric softening compositions prepared in comparative example 1, comparative example 2 and example 1, example 2 were tested for the detergency effect on detergents in the recommended concentration range, the water amount in the main wash stage of machine washing was 20L, the solid fabric softening composition of the present invention was recommended to be used in a single dose of 8 to 16g, comparative example 1 was recommended to be used in a single dose of 20 to 40g, comparative example 2 was recommended to be used in a single dose of 40 to 80g, and the comparative example and example were evaluated for the detergency effect by adding the same amount of detergent (0.2%) and the detergent was selected from the commercially available general detergents (in this test, a fragrance-free liquid laundry detergent of up Bai Quan effect) in the test method as described, and the results are shown in table 5:

TABLE 5 detergency impact test results

The larger the national standard P value is, the smaller the influence on decontamination is; when only detergents are used, the decontamination ratio P of the national standard carbon black dirt cloth, the protein dirt cloth and the sebum dirt cloth is higher, and the samples of the comparative example and the example are added to have different degrees of influence on the national standard decontamination. Comparative example 1 has a relatively significant negative effect on the decontamination P value at a single recommended dosage of 20g, i.e., at a test concentration of 0.1%; the drop in the decontamination P value is very pronounced at the recommended level of 40g, i.e., at a test concentration of 0.2%; in other words, the effect on national standard decontamination is proportional to the increase in usage. The same trend exists for the effects of comparative example 2 and comparative example 1 on national standard soil release, but comparative example 1 is not significant. The influence of the example 1 and the example 2 on the national standard decontamination is not obvious in the comparative example 1 and the comparative example 2, the influence is not obviously increased along with the increase of the dosage, and particularly, the influence on the cleaning power of the national standard protein dirt cloth and the national standard sebum dirt cloth is small, and the influence on the decontamination is judged to be no, so that the detergent meets the requirements of consumers on the compliant product used together with the laundry detergent.

3. Formability test

Comparative example 4 and comparative example 5 are commercially available laundry fragrance-retaining beads with polyethylene glycol PEG as the water-soluble carrier, as is well known in the art.

Comparative example 3 and examples 4-9 formulation methods were as described, the ratio q was measured as described, and the specific components and contents were as shown in table 6:

TABLE 6 composition and evaluation grade of solid fabric softening compositions of examples 4-9

Comparative example 3 without the addition of a forming aid fatty alcohol, the particle forming size ratio q was 0.41, and the addition of fatty alcohol changed the surface properties of the composition so that the contact angle with the steel strip was reduced, and the resulting particles were flat hemispherical particles approaching hemispherical shapes. The proportion of fatty alcohol in the composition is 0.5% -3.5%, the granule forming property is optimal, and the granule forming property is far better than that of comparative example 4 and comparative example 5 which are commercial products, and is also better than that of comparative example 3 without fatty alcohol.

4. Odor assessment test

The formulation methods of comparative example 6 and examples 10-18 were as described, the evaluation method of odor stability was as described, the higher the average score, the better the odor stability, and the specific components and contents were as shown in table 7:

TABLE 7 composition and odor stability score for solid fabric softening compositions of examples 10-18

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In the above embodiments, the addition of the aminocarboxylic acid chelating agent EDTA salt, the EDTMPS of the organophosphonic acid and the HEDP salt effectively improves the compatibility of the solid softening composition with the PVA water-soluble film, wherein it has surprisingly been found that the HEDP sodium salt, particularly HEDP-2Na, significantly improves the compatibility of the softening composition with the polyvinyl alcohol PVA water-soluble film, particularly with respect to the retention of odor note and intensity after long-term storage, and significantly reduces subjective language descriptions of volunteers such as fishy smell, malodor, sour taste and plastic taste.

Compared with the prior art, the invention has the beneficial effects that:

1. the invention adopts polyethylene glycol as a water-soluble carrier, selects a cationic polymer with a special structure as a fabric softener, and puts the cationic polymer, the fabric and the detergent into a washing machine cylinder together, and the cationic polymer, the fabric and the fabric are subjected to rinsing in a main washing stage, so that the fabric has obvious perceivable softening effect and the detergency of the detergent is not reduced.

2. The fatty alcohol is used as a forming auxiliary agent, so that the method can be widely applied to different essences, and the difference of different PEG molecular weights and molecular weight distribution on slurry is caused. The shape of the particles can be adjusted according to different formulas to produce particles with plump desired size.

3. The chelating agent is used as the fragrance stabilizing auxiliary agent, so that the compatibility of the solid particles and the polyvinyl alcohol water-soluble film is improved, and the stability of the odor between the polyethylene glycol PEG perfuming particle composition and the water-soluble film is obviously improved.

Claims

1. A solid fabric softening composition, characterized in that the composition consists of: 40-95% of polyethylene glycol, 0.5-5% of cationic polymer, 0.01-5% of fragrance stabilizing auxiliary agent, 0.1-5% of forming auxiliary agent, 0.1-15% of spice and 0.01-30% of other auxiliary agents; the side chain of the cationic polymer contains polyoxyethylene groups, and the average ethoxylation degree is 1-20; the forming auxiliary agent is fatty alcohol;

the molecular weight of the polyethylene glycol is 4000-8000, the weight average molecular weight of the cationic polymer is 100000-1000000, and the fatty alcohol is one or a mixture of a plurality of C14-C18 fatty alcohols;

the cationic polymer is a cellulose polymer comprising quaternary ammonium groups;

the fragrance stabilizing auxiliary agent is one or a mixture of more than one of ethylenediamine tetraacetate, ethylenediamine tetramethylene phosphonate and hydroxyethylidene bisphosphonate.