CN112725098B - Microcapsule essence laundry detergent and preparation method thereof - Google Patents
Microcapsule essence laundry detergent and preparation method thereof Download PDFInfo
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- CN112725098B CN112725098B CN202011579147.2A CN202011579147A CN112725098B CN 112725098 B CN112725098 B CN 112725098B CN 202011579147 A CN202011579147 A CN 202011579147A CN 112725098 B CN112725098 B CN 112725098B
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- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0007—Aliphatic compounds
- C11B9/0015—Aliphatic compounds containing oxygen as the only heteroatom
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0007—Aliphatic compounds
- C11B9/0023—Aliphatic compounds containing nitrogen as the only heteroatom
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- 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
- C11D3/16—Organic compounds
- C11D3/24—Organic compounds containing halogen
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- 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
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/32—Amides; Substituted amides
- C11D3/323—Amides; Substituted amides urea or derivatives thereof
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- 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
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
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- 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
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/378—(Co)polymerised monomers containing sulfur, e.g. sulfonate
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- 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
- C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
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- 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
- C11D3/50—Perfumes
- C11D3/502—Protected perfumes
- C11D3/505—Protected perfumes encapsulated or adsorbed on a carrier, e.g. zeolite or clay
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- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
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- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
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Abstract
The invention belongs to the field of laundry detergent, and relates to a microcapsule essence laundry detergent and a preparation method thereof. The microcapsule essence laundry detergent contains sorbitan fatty acid ester, alkyl sodium sulfonate, acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer, polysiloxane, microcapsule essence, a bactericide and deionized water; the microcapsule essence consists of a wall material and a core material, wherein the wall material is polyurea resin, and the core material is prepared from the following raw materials in percentage by weight: 1-5% of tea tree essential oil, 3-6% of eucalyptus oil, 0.5-1% of rose essential oil, 30-40% of p-tert-butylcyclohexyl acetate, 2-6% of ethyl naphthyl ether, 5-10% of tricyclodecenyl acetate, 8-12% of isopropyl myristate, 1-5% of dodecanonitrile and 1-5% of dodecanal. The microcapsule essence laundry detergent provided by the invention can delay the sedimentation of the microcapsule essence.
Description
Technical Field
The invention belongs to the field of laundry detergent, and particularly relates to a microcapsule essence laundry detergent and a preparation method thereof.
Background
The microcapsule essence is a very tiny saccular substance formed by taking a high molecular compound as a wall material and encapsulating the required essence in the wall material. The microcapsule essence is favored by consumers due to good slow release property. Microcapsule essence is added into the laundry detergent, and when the obtained microcapsule essence laundry detergent is used for washing clothes, the capsule wall of the microcapsule essence is gradually broken due to friction between clothes and between the clothes and rolling in the washing machine, so that the fragrance retaining effect is achieved.
In addition, the microcapsule essence particles in the microcapsule essence laundry detergent are initially in a suspended state, but due to the influence of gravity and interfacial energy, the microcapsule essence particles are aggregated and settled along with the prolonging of storage and gradually settle at the bottom of the laundry detergent, so that the use effect is influenced. Therefore, there is an urgent need to develop a laundry detergent that can avoid or delay the precipitation of microcapsule perfume particles.
Disclosure of Invention
The invention aims to overcome the defect that the microcapsule essence in the existing microcapsule essence laundry detergent can aggregate and settle along with the prolonging of the storage time, and provides the microcapsule essence laundry detergent capable of delaying the settlement of the microcapsule essence and the preparation method thereof.
The microcapsule essence laundry detergent contains sorbitan fatty acid ester, sodium alkylsulfonate, acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer, polysiloxane, microcapsule essence, a bactericide and deionized water; the microcapsule essence is composed of a wall material and a core material, wherein the wall material is polyurea resin, and the core material is prepared from the following raw materials in percentage by weight based on the total weight of the microcapsule essence: 1-5% of tea tree essential oil, 3-6% of eucalyptus oil, 0.5-1% of rose essential oil, 30-40% of p-tert-butylcyclohexyl acetate, 2-6% of ethyl naphthyl ether, 5-10% of tricyclodecenyl acetate, 8-12% of isopropyl myristate, 1-5% of dodecanonitrile and 1-5% of dodecanal; the mass ratio of the sorbitan fatty acid ester, the alkyl sodium sulfonate, the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer and the polysiloxane is (0.1-0.5): 5-10): 1-3): 1.
Preferably, the total weight of the microcapsule essence laundry detergent is taken as a reference, the total content of the sorbitan fatty acid ester, the sodium alkylsulfonate, the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer and the polysiloxane is 20-50 wt%, the content of the microcapsule essence is 0.1-5 wt%, the content of the bactericide is 0.1-2 wt%, and the balance is deionized water.
Preferably, the mol ratio of the acrylamide structural unit to the 2-acrylamide-2-methylpropanesulfonic acid structural unit in the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer is (2-4): 1.
Preferably, the number average molecular weight of the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer is 1000-5000.
Preferably, the sorbitan fatty acid ester is selected from at least one of sorbitan monolaurate (span 20), sorbitan monopalmitate (span 40), sorbitan monostearate (span 60), sorbitan tristearate (span 65) and sorbitan trioleate (span 85).
Preferably, the sodium alkylsulfonate is selected from at least one of sodium dodecylsulfonate, sodium hexadecylsulfonate and sodium octadecylsulfonate.
Preferably, the polysiloxane has a number average molecular weight of 1000 to 3000.
Preferably, the bactericide is at least one selected from the group consisting of 4, 4-dichloro-2-hydroxydiphenyl ether (HP-100), 4-chloro-3, 5-xylenol (PCMX), 3,4, 4-Trichlorocarbanilide (TCC) and 2,4, 4' -trichloro-2-hydroxydiphenyl ether (TCS).
Preferably, the particle size of the microcapsule essence is 10-30 μm.
Preferably, the polyurea resin has a number average molecular weight of 1000 to 6000.
Preferably, the microcapsule essence is prepared by the following steps:
s1, adding ethyl naphthyl ether into p-tert-butylcyclohexyl acetate with the mass being 2-5 times that of the ethyl naphthyl ether, stirring and heating to 50-60 ℃, keeping for a period of time to enable the ethyl naphthyl ether to be completely dissolved, and then standing and cooling to room temperature to obtain an ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound;
s2, under the stirring condition, slowly adding tea tree essential oil, eucalyptus oil, rose essential oil, tricyclodecenyl acetate, isopropyl myristate, dodecanonitrile, dodecanal and the rest p-tert-butylcyclohexyl acetate into a container in sequence according to the sequence of nitrile, ester, aldehyde and oil, stirring and mixing uniformly, then slowly adding the ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound obtained in the step S1, continuously stirring and mixing uniformly, and standing for 20-30 hours to obtain a core material;
s3, uniformly stirring and mixing the polyurea resin and the core material, and then carrying out spray drying on the obtained mixture to obtain the microcapsule essence.
In addition, the invention also provides a preparation method of the microcapsule essence laundry detergent, which comprises the following steps:
s1, adding ethyl naphthyl ether into p-tert-butylcyclohexyl acetate with the mass being 2-5 times that of the ethyl naphthyl ether, stirring and heating to 50-60 ℃, keeping for a period of time to enable the ethyl naphthyl ether to be completely dissolved, and then standing and cooling to room temperature to obtain an ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound;
s2, under the stirring condition, slowly adding tea tree essential oil, eucalyptus oil, rose essential oil, tricyclodecenyl acetate, isopropyl myristate, dodecanonitrile, dodecanal and the rest p-tert-butylcyclohexyl acetate into a container in sequence according to the sequence of nitrile, ester, aldehyde and oil, stirring and mixing uniformly, then slowly adding the ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound obtained in the step S1, continuously stirring and mixing uniformly, and standing for 20-30 hours to obtain a core material;
s3, uniformly stirring and mixing the polyurea resin and the core material, and then carrying out spray drying on the obtained mixture to obtain the microcapsule essence;
s4, uniformly stirring and mixing the microcapsule essence, sorbitan fatty acid ester, sodium alkyl sulfonate, acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer, polysiloxane, bactericide and deionized water.
Preferably, in step S1, the heating rate is 0.5-1 ℃/min.
Preferably, in step S2, the stirring conditions include a rotation speed of 100 to 1000r/min and a stirring time of 0.5 to 1 hour after the raw material is added.
Preferably, in step S2, the dodecanitrile is added to the container at one time, and the addition rate of each of the other raw materials is 0.2 to 2g/min with respect to 1g of dodecanitrile.
Preferably, in the step S3, the spray drying conditions include a spray inlet air temperature of 140-170 ℃, an outlet air temperature of 80-95 ℃, an atomizer frequency of 165-200 Hz, a cooling air temperature of 16-22 ℃ and a feeding temperature of 50-60 ℃.
After extensive and intensive research, the inventor of the invention finds that when the microcapsule essence laundry detergent contains the sorbitan fatty acid ester, the sodium alkylsulfonate, the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer and the polysiloxane in a specific ratio, and the microcapsule essence takes the polyurea resin as a wall material, the microcapsule essence in the microcapsule essence laundry detergent can be stably suspended in the laundry detergent for a long time, so that the sedimentation of the microcapsule essence can be effectively delayed, and the storage stability of the obtained microcapsule essence laundry detergent is very good.
The inventor of the invention also finds that when the microcapsule essence takes polyurea resin as a wall material, 1-5% of tea tree essential oil, 3-6% of eucalyptus oil, 0.5-1% of rose essential oil, 30-40% of p-tert-butylcyclohexyl acetate, 2-6% of ethyl naphthyl ether, 5-10% of tricyclodecenyl acetate, 8-12% of isopropyl myristate, 1-5% of dodecanonitrile and 1-5% of dodecanal are compounded as a core material, in the microcapsule forming process, the ethyl naphthyl ether is recrystallized in the acetic acid p-tert-butylcyclohexyl ester to form an ethyl naphthyl ether/acetic acid p-tert-butylcyclohexyl ester compound, and then the core material is formed according to the sequential mixing of nitrile, ester, aldehyde, oil and the ethyl naphthyl ether/acetic acid p-tert-butylcyclohexyl ester compound, the specific core material mixing sequence can enable each component of the core material to realize the molecular-level compounding, and the obtained microcapsule essence is easier to suspend in the laundry detergent, and the storage stability is better.
Detailed Description
In the microcapsule essence provided by the invention, the content of the Tea tree essential oil (Tea tree oil) is 1-5%, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5% and the like. The content of the eucalyptus oil (eucalyptus oil) is 3 to 6%, for example, may be 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, or the like. The content of the rose essential oil (rose essential oil) is 0.5-1%, for example, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, etc. The content of the p-tert-butylcyclohexyl acetate (ptbcha) is 30 to 40%, and for example, may be 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, or the like. The content of the ethyl naphthyl ether (neroli broomelia) is 2 to 6%, and may be, for example, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, or the like. The content of tricyclodecenyl acetate (cyclet) is 5 to 10%, and may be, for example, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, or 8%.5%, 9%, 9.5%, 10%, etc. The content of isopropyl myristate (IPM) is 8 to 12%, and for example, may be 8%, 9%, 10%, 11%, 12% or the like. The content of the dodecanonitrile (clonal) is 1 to 5%, and may be, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or the like. The dodecanal (ald C)12) The content of (b) is 1 to 5%, and for example, may be 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, etc.
In the most preferred embodiment of the present invention, the core material is made of the following raw materials in percentage by weight: 2.5 percent of tea tree essential oil, 4.5 percent of eucalyptus oil, 0.7 percent of rose essential oil, 34.5 percent of p-tert-butylcyclohexyl acetate, 3.5 percent of ethyl naphthyl ether, 7.5 percent of tricyclodecenyl acetate, 9.5 percent of isopropyl myristate, 2.5 percent of dodecanonitrile and 2.5 percent of dodecanal.
In the invention, the particle size of the microcapsule essence is preferably 10-30 μm, for example, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm and the like.
The present invention will be described in detail below by way of examples. The examples of embodiments are intended to be illustrative of the invention and are not to be construed as limiting the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
(1) Preparing microcapsule essence:
the microcapsule essence adopted in this embodiment is composed of a wall material and a core material, the wall material is polyurea resin (number average molecular weight is 3000, the same below), and the core material is prepared from the following raw materials in percentage by weight based on the total weight of the microcapsule essence: 2.5 percent of tea tree essential oil, 4.5 percent of eucalyptus oil, 0.7 percent of rose essential oil, 34.5 percent of p-tert-butylcyclohexyl acetate, 3.5 percent of ethyl naphthyl ether, 7.5 percent of tricyclodecenyl acetate, 9.5 percent of isopropyl myristate, 2.5 percent of dodecanonitrile and 2.5 percent of dodecanal. The microcapsule essence is prepared by the following method:
s1, adding ethyl naphthyl ether into p-tert-butylcyclohexyl acetate with the mass 2 times that of the p-tert-butylcyclohexyl acetate, heating to 55 ℃ at the speed of 1 ℃/min under the stirring condition, keeping for a period of time to completely dissolve the ethyl naphthyl ether, and then standing and cooling to room temperature to obtain an ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound;
s2, under the condition of stirring (the rotating speed is 500r/min, the same below), tea tree essential oil, eucalyptus oil, rose essential oil, tricyclodecenyl acetate, isopropyl myristate, dodecanonitrile, dodecanal and the rest of p-tert-butylcyclohexyl acetate are slowly added into a container according to the sequence of nitrile, ester, aldehyde and oil, the adding speed of the rest of raw materials is 0.2g/min relative to 1g of dodecanonitrile, the raw materials are stirred for 30min after being added so as to uniformly mix the components, then the ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound obtained in the step S1 is slowly added at the speed of 0.2g/min, the mixture is continuously stirred and uniformly mixed, and the core material is obtained after standing for 25 h;
s3, uniformly stirring and mixing the polyurea resin and the core material, introducing the obtained mixture into spray drying equipment, controlling the air inlet temperature at 150 ℃, the air outlet temperature at 90 ℃, the frequency of an atomizer at 180Hz, the cooling air temperature at 20 ℃, and the feeding temperature at 55 ℃ to obtain the microcapsule essence (marked as WJ-1) with the particle size of 10-30 microns.
(2) Preparing a microcapsule essence laundry detergent:
uniformly stirring and mixing sorbitan monolaurate, sodium dodecyl sulfate, an acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer (the number average molecular weight is 2000, wherein the molar ratio of an acrylamide structural unit to a 2-acrylamide-2-methylpropanesulfonic acid structural unit is 3:1) and polysiloxane (the number average molecular weight is 2000) according to the mass ratio of 0.3:8:2:1, uniformly stirring and mixing the obtained mixture, microcapsule essence WJ-1, HP-100 and water to obtain a microcapsule essence laundry detergent, wherein the content of the microcapsule essence in the laundry detergent is 3 wt%, and the total content of the sorbitan monolaurate, the sodium dodecyl sulfate, the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer and the polysiloxane is 40 wt%, HP-100 in an amount of 0.5 wt%, with the balance being water.
Example 2
(1) Preparing microcapsule essence:
the microcapsule essence adopted in the embodiment comprises a wall material and a core material, wherein the wall material is polyurea resin, and the core material is prepared from the following raw materials in percentage by weight based on the total weight of the microcapsule essence: tea tree essential oil 2%, eucalyptus oil 3%, rose essential oil 1%, p-tert-butylcyclohexyl acetate 30%, ethyl naphthyl ether 2%, tricyclodecenyl acetate 10%, isopropyl myristate 12%, dodecanonitrile 2.5% and dodecanal 2.5%. The microcapsule essence is prepared by the following method:
s1, adding ethyl naphthyl ether into p-tert-butylcyclohexyl acetate with the mass 2.5 times that of the p-tert-butylcyclohexyl acetate, heating to 55 ℃ at the speed of 1 ℃/min under the stirring condition, keeping for a period of time to completely dissolve the ethyl naphthyl ether, and then standing and cooling to room temperature to obtain an ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound;
s2, under the stirring condition, adding tea tree essential oil, eucalyptus oil, rose essential oil, tricyclodecenyl acetate, isopropyl myristate, dodecanonitrile, dodecanal and the rest p-tert-butylcyclohexyl acetate into a container slowly in sequence according to the sequence of nitrile, ester, aldehyde and oil, wherein the adding speed of the rest raw materials is 0.5g/min relative to 1g of dodecanonitrile, stirring for 30min after the raw materials are added to uniformly mix the components, then slowly adding the ethyl naphthyl ether/acetic acid p-tert-butylcyclohexyl compound obtained in the step S1 at the speed of 0.5g/min, continuously stirring and uniformly mixing, and standing for 25h to obtain a core material;
s3, uniformly stirring and mixing the polyurea resin and the core material, introducing the obtained mixture into spray drying equipment, controlling the air inlet temperature at 150 ℃, the air outlet temperature at 90 ℃, the frequency of an atomizer at 180Hz, the cooling air temperature at 20 ℃, and the feeding temperature at 55 ℃ to obtain the microcapsule essence (marked as WJ-2) with the particle size of 10-30 microns.
(2) Preparing a microcapsule essence laundry detergent:
uniformly stirring and mixing sorbitan monolaurate, sodium dodecyl sulfate, an acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer (the number average molecular weight is 2000, wherein the molar ratio of an acrylamide structural unit to a 2-acrylamide-2-methylpropanesulfonic acid structural unit is 3:1) and polysiloxane (the number average molecular weight is 2000) according to the mass ratio of 0.3:8:2:1, then uniformly stirring and mixing the obtained mixture, microcapsule essence WJ-2, HP-100 and water to obtain the microcapsule essence laundry detergent, wherein the content of the microcapsule essence in the laundry detergent is 0.1 wt%, and the total content of the sorbitan monolaurate, the sodium dodecyl sulfate, the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer and the polysiloxane is 20 wt%, HP-100 in an amount of 0.1 wt%, with the balance being water.
Example 3
(1) Preparing microcapsule essence:
the microcapsule essence adopted in the embodiment comprises a wall material and a core material, wherein the wall material is polyurea resin, and the core material is prepared from the following raw materials in percentage by weight based on the total weight of the microcapsule essence: 3% of tea tree essential oil, 6% of eucalyptus oil, 0.5% of rose essential oil, 40% of p-tert-butylcyclohexyl acetate, 6% of ethyl naphthyl ether, 5% of tricyclodecenyl acetate, 8% of isopropyl myristate, 2.5% of dodecanonitrile and 2.5% of dodecanaldehyde. The microcapsule essence is prepared by the following method:
s1, adding ethyl naphthyl ether into p-tert-butylcyclohexyl acetate with the mass being 3 times that of the p-tert-butylcyclohexyl acetate, heating to 55 ℃ at the speed of 1 ℃/min under the stirring condition, keeping for a period of time to completely dissolve the ethyl naphthyl ether, and then standing and cooling to room temperature to obtain an ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound;
s2, under the stirring condition, adding tea tree essential oil, eucalyptus oil, rose essential oil, tricyclodecenyl acetate, isopropyl myristate, dodecanonitrile, dodecanal and the rest p-tert-butylcyclohexyl acetate into a container slowly in sequence according to the sequence of nitrile, ester, aldehyde and oil, wherein the adding speed of the rest raw materials is 1g/min relative to 1g of dodecanonitrile, stirring for 30min after the raw materials are added to uniformly mix the components, slowly adding the ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound obtained in the step S1 at the speed of 1g/min, continuously stirring and uniformly mixing, and standing for 25h to obtain a core material;
s3, uniformly stirring and mixing the polyurea resin and the core material, introducing the obtained mixture into spray drying equipment, controlling the air inlet temperature at 150 ℃, the air outlet temperature at 90 ℃, the frequency of an atomizer at 180Hz, the cooling air temperature at 20 ℃, and the feeding temperature at 55 ℃ to obtain the microcapsule essence (marked as WJ-3) with the particle size of 10-30 microns.
(2) Preparing a microcapsule essence laundry detergent:
uniformly stirring and mixing sorbitan monolaurate, sodium dodecyl sulfate, an acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer (the number average molecular weight is 2000, wherein the molar ratio of an acrylamide structural unit to a 2-acrylamide-2-methylpropanesulfonic acid structural unit is 3:1) and polysiloxane (the number average molecular weight is 2000) according to the mass ratio of 0.3:8:2:1, uniformly stirring and mixing the obtained mixture, microcapsule essence WJ-3, HP-100 and water to obtain a microcapsule essence laundry detergent, wherein the content of the microcapsule essence in the laundry detergent is 5 wt%, and the total content of the sorbitan monolaurate, the sodium dodecyl sulfate, the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer and the polysiloxane is 50 wt%, HP-100 in an amount of 2 wt%, with the balance being water.
Example 4
Preparing microcapsule essence and microcapsule laundry detergent according to the method of example 3, except that step S1 is not included in the preparation process of microcapsule essence, but all core materials are slowly added into a container in sequence of nitrile, ester, aldehyde and oil, and are uniformly stirred and mixed, and the rest conditions are the same as those in example 3, so as to obtain the reference microcapsule essence and the reference microcapsule essence laundry detergent.
Comparative example 1
The microcapsule essence and microcapsule essence laundry liquid were prepared according to the method of example 4, except that sodium dodecyl sulfate was replaced with sorbitan monolaurate in the same weight part, and the other conditions were the same as in example 4, to obtain the reference microcapsule essence and microcapsule essence laundry liquid.
Comparative example 2
The microcapsule essence and microcapsule essence laundry liquid were prepared according to the method of example 4, except that the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer was replaced with the same weight part of polyacrylamide (number average molecular weight 2000), and the rest of the conditions were the same as those of example 4, to obtain the reference microcapsule essence and microcapsule essence laundry liquid.
Comparative example 3
A microcapsule essence and a microcapsule laundry detergent were prepared according to the method of example 4, except that the polysiloxane was replaced with sorbitan monolaurate in the same weight part, and the rest conditions were the same as in example 4, to obtain a reference microcapsule essence and microcapsule laundry detergent.
Comparative example 4
The microcapsule essence and the microcapsule laundry detergent are prepared according to the method of example 4, except that p-tert-butylcyclohexyl acetate is replaced by the same mass part of rose alcohol, and the rest conditions are the same as those of example 4, so as to obtain the reference microcapsule essence and microcapsule laundry detergent.
Comparative example 5
The microcapsule essence and the microcapsule laundry detergent are prepared according to the method of example 4, except that in the preparation process of the microcapsule essence, the polyurea resin is replaced by the same weight part of chitosan, and the rest conditions are the same as those of example 4, so as to obtain the reference microcapsule essence and the microcapsule laundry detergent.
Test example
And respectively carrying out centrifugal separation on 1L of the microcapsule essence laundry liquid prepared just in examples 1-4 and the reference microcapsule essence laundry liquid prepared just in comparative examples 1-5, carrying out suspension dispersion-centrifugal separation on the obtained solid product again by adopting water, repeatedly treating for three times, and drying the solid product, wherein the weight of the obtained product is recorded as M1.
Respectively storing 1L of the microcapsule essence laundry liquid obtained in the embodiments 1-4 and the reference microcapsule essence laundry liquid obtained in the comparative examples 1-5 in a separating funnel with a piston at the bottom in a sealing manner for 2 years, then releasing 100mL of the microcapsule essence laundry liquid from the bottom of the separating funnel, centrifugally separating the part of the laundry liquid, performing suspension dispersion-centrifugal separation again on the obtained solid product by adopting water, repeating the treatment for three times, and drying the solid product, wherein the weight of the obtained product is recorded as M2. The precipitation rate D was calculated according to the following equation (M2-1/10M1)/M1 × 100%. The results are shown in Table 1.
TABLE 1
| Item | Precipitation Rate (%) |
| Example 1 | 0.5％ |
| Example 2 | 0.3％ |
| Example 3 | 0.9％ |
| Example 4 | 5.8％ |
| Comparative example 1 | 10.6％ |
| Comparative example 2 | 11.1％ |
| Comparative example 3 | 10.4％ |
| Comparative example 4 | 12.9％ |
| Comparative example 5 | 10.6％ |
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (8)
1. The microcapsule essence laundry detergent is characterized by comprising sorbitan fatty acid ester, alkyl sodium sulfonate, acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer, polysiloxane, microcapsule essence, a bactericide and deionized water; the microcapsule essence is composed of a wall material and a core material, wherein the wall material is polyurea resin, and the core material is prepared from the following raw materials in percentage by weight based on the total weight of the microcapsule essence: 1-5% of tea tree essential oil, 3-6% of eucalyptus oil, 0.5-1% of rose essential oil, 30-40% of p-tert-butylcyclohexyl acetate, 2-6% of ethyl naphthyl ether, 5-10% of tricyclodecenyl acetate, 8-12% of isopropyl myristate, 1-5% of dodecanonitrile and 1-5% of dodecanal; the mass ratio of the sorbitan fatty acid ester, the alkyl sodium sulfonate, the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer and the polysiloxane is (0.1-0.5): 5-10): 1-3): 1; the microcapsule essence is prepared by the following steps:
s1, adding ethyl naphthyl ether into p-tert-butylcyclohexyl acetate with the mass being 2-5 times that of the ethyl naphthyl ether, stirring and heating to 50-60 ℃, keeping for a period of time to enable the ethyl naphthyl ether to be completely dissolved, and then standing and cooling to room temperature to obtain an ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound;
s2, under the stirring condition, slowly adding tea tree essential oil, eucalyptus oil, rose essential oil, tricyclodecenyl acetate, isopropyl myristate, dodecanonitrile, dodecanal and the rest p-tert-butylcyclohexyl acetate into a container in sequence according to the sequence of nitrile, ester, aldehyde and oil, stirring and mixing uniformly, then slowly adding the ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound obtained in the step S1, continuously stirring and mixing uniformly, and standing for 20-30 hours to obtain a core material;
s3, uniformly stirring and mixing the polyurea resin and the core material, and then carrying out spray drying on the obtained mixture to obtain the microcapsule essence.
2. The microcapsule essence laundry detergent of claim 1, wherein the total content of the sorbitan fatty acid ester, the sodium alkylsulfonate, the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer and the polysiloxane is 20-50 wt%, the content of the microcapsule essence is 0.1-5 wt%, the content of the bactericide is 0.1-2 wt%, and the balance is deionized water, based on the total weight of the microcapsule essence laundry detergent.
3. The microcapsule essence laundry detergent according to claim 1, wherein the molar ratio of the acrylamide structural unit to the 2-acrylamide-2-methylpropanesulfonic acid structural unit in the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer is (2-4): 1; the number average molecular weight of the acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer is 1000-5000.
4. The microcapsule perfume laundry detergent of claim 1, wherein the sorbitan fatty acid ester is selected from at least one of sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan tristearate, and sorbitan trioleate; the sodium alkyl sulfonate is selected from at least one of sodium dodecyl sulfonate, sodium hexadecyl sulfonate and sodium octadecyl sulfonate; the number average molecular weight of the polysiloxane is 1000-3000; the bactericide is selected from at least one of 4, 4-dichloro-2-hydroxydiphenyl ether, 4-chloro-3, 5-xylenol, 3,4, 4-trichloro-sym-diphenyl urea and 2,4, 4' -trichloro-2-hydroxydiphenyl ether.
5. The microcapsule essence laundry detergent of claim 1, wherein the microcapsule essence has a particle size of 10-30 μm.
6. The microcapsule essence laundry detergent of claim 1, wherein the polyurea resin has a number average molecular weight of 1000-6000.
7. The microcapsule essence laundry detergent according to claim 1, characterized in that,
in the step S1, the heating rate is 0.5-1 ℃/min;
in the step S2, the stirring conditions include that the rotating speed is 100-1000 r/min, and the stirring time after the raw material is added is 0.5-1 h;
in the step S2, adding the dodecanitrile into a container at one time, wherein the adding speed of the rest raw materials is 0.2-2 g/min relative to 1g of dodecanitrile;
in the step S3, the spray drying conditions include a spray inlet air temperature of 140-170 ℃, an outlet air temperature of 80-95 ℃, an atomizer frequency of 165-200 Hz, a cooling air temperature of 16-22 ℃, and a feeding temperature of 50-60 ℃.
8. The preparation method of the microcapsule essence laundry detergent as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
s1, adding ethyl naphthyl ether into p-tert-butylcyclohexyl acetate with the mass being 2-5 times that of the ethyl naphthyl ether, stirring and heating to 50-60 ℃, keeping for a period of time to enable the ethyl naphthyl ether to be completely dissolved, and then standing and cooling to room temperature to obtain an ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound;
s2, under the stirring condition, slowly adding tea tree essential oil, eucalyptus oil, rose essential oil, tricyclodecenyl acetate, isopropyl myristate, dodecanonitrile, dodecanal and the rest p-tert-butylcyclohexyl acetate into a container in sequence according to the sequence of nitrile, ester, aldehyde and oil, stirring and mixing uniformly, then slowly adding the ethyl naphthyl ether/p-tert-butylcyclohexyl acetate compound obtained in the step S1, continuously stirring and mixing uniformly, and standing for 20-30 hours to obtain a core material;
s3, uniformly stirring and mixing the polyurea resin and the core material, and then carrying out spray drying on the obtained mixture to obtain the microcapsule essence;
s4, uniformly stirring and mixing the microcapsule essence, sorbitan fatty acid ester, sodium alkyl sulfonate, acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer, polysiloxane, bactericide and deionized water.
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| KR20080084233A (en) * | 2007-03-15 | 2008-09-19 | 양환승 | Spray system of laundry treatment device for spraying silver nano or aromatic microcapsules |
| CN105647678A (en) * | 2016-01-14 | 2016-06-08 | 广州立白企业集团有限公司 | Method for improving protein dirt removing capability of washing agent composition and washing agent composition |
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| CN109679779A (en) * | 2018-12-14 | 2019-04-26 | 广州市骅香生物科技有限公司 | A kind of micro-sachet liquid detergent and preparation method thereof |
| CN110734815B (en) * | 2019-10-18 | 2021-06-04 | 广州大白生物科技有限公司 | Microcapsule essence laundry detergent and preparation method thereof |
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| CN105647678A (en) * | 2016-01-14 | 2016-06-08 | 广州立白企业集团有限公司 | Method for improving protein dirt removing capability of washing agent composition and washing agent composition |
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