CN116726544B - Fragrance retaining agent and preparation method and application thereof - Google Patents

Fragrance retaining agent and preparation method and application thereof Download PDF

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Publication number
CN116726544B
CN116726544B CN202310785348.5A CN202310785348A CN116726544B CN 116726544 B CN116726544 B CN 116726544B CN 202310785348 A CN202310785348 A CN 202310785348A CN 116726544 B CN116726544 B CN 116726544B
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reaction kettle
fragrance
essence
molecular sieve
zeolite molecular
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CN116726544A (en
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李轩光
卢少萍
冯学泉
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Qingdao Chuntian Food Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/30Accessories for evaporators ; Constructional details thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/0007Aliphatic compounds
    • C11B9/0015Aliphatic compounds containing oxygen as the only heteroatom
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/005Compositions containing perfumes; Compositions containing deodorants
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Textile Engineering (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention relates to a fragrance retention agent and a preparation method and application thereof, wherein the fragrance retention agent comprises high-concentration essence prepared by a special process, the essence is concentrated by adopting a zeolite molecular sieve under a heating condition after being mixed with a solvent, and then ethanol is further adopted for a dealcoholization step.

Description

Fragrance retaining agent and preparation method and application thereof
Technical Field
The invention belongs to the technical field of essence and spice, and particularly relates to a fragrance retaining agent, a preparation method and application thereof.
Background
Along with the improvement of living standard of people, pursuit of people on material life is diversified, and wearing requirements of people on clothes in daily life are not only simply reflected in attractive appearance, but also higher and higher requirements on fragrance, fragrance retention time and the like of the clothes, so that more and more fragrances and essences are developed into various forms suitable for different places to meet the requirements of different places.
When the general perfume is stored or processed into an aromatic product, the perfume is exposed to the environment, so that the perfume components volatilize rapidly, the perfume keeping time is short, the perfume is easily oxidized due to contact with air in a large area, the perfume is deteriorated, and the quality guarantee period is short, so that the conventional method and means for overcoming the technical difficulty mainly wrap the volatile components, such as perfume microcapsules, wrap perfume core materials through wall materials, and play a role in slow release and protection on the perfume, but the preparation method of the perfume microcapsules is generally complex and complicated, the embedding rate is difficult to reach the standard, and the microcapsules are easy to adhere to the capsule cores and the capsule walls after long-term storage, so that the normal use is difficult, and the effect is poor, such as patent CN109652215A, CN 113563987A. Therefore, developing a high concentration of perfume is another effective means to solve the problem of poor perfume retention from the source.
The prior production method of the high-concentration essence comprises expensive production technologies such as permeable membrane technology, macroporous resin adsorption and the like, is complicated in process, is difficult to realize industrial production, and further comprises the steps of directly adding porous materials such as active carbon, kaolin, zeolite, bentonite and the like into a product, adsorbing volatile substances through a porous material channel, further slowly releasing aroma to achieve a better release effect.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a fragrance retention agent, a preparation method and application thereof, and the fragrance retention agent with high concentration essence obtained by the preparation obtains better fragrance retention effect, is suitable for industrial production and has wide application prospect.
In a first aspect, the invention provides a preparation method of high-concentration essence, which specifically comprises the following steps:
s1, adding perfume and solvent into a jacketed reaction kettle, heating the reaction kettle to 60-90 ℃, and stirring for 0.5-1 hour;
S2, adding zeolite molecular sieve into the reaction kettle, wherein the zeolite molecular sieve accounts for 5-20% of the mass of the materials in the reaction kettle, adjusting the pH value to 4.5-6, stirring for 1-5 hours, cooling, filtering, and filtering out liquid;
and S3, adding an ethanol solution into a reaction kettle only containing zeolite molecular sieve, continuously heating the reaction kettle to 60-90 ℃, filtering, and concentrating the filtrate to obtain the high-concentration essence.
Further, the raw material sources of the perfume of the present invention include, but are not limited to, one or more of jasmine, rosemary, lavender, lily, rose, gardenia, orange peel or concentrated juice.
In a second aspect, the invention also provides the high-concentration essence prepared by the preparation method of the high-concentration essence.
In a third aspect, the present invention also provides a high-power essence fragrance-retaining agent, which further comprises one or more components selected from alcohols, ethers, natural polysaccharides and adjuvants.
Further, the alcohol is selected from polyvinyl alcohol or polyethylene glycol.
Further, the ethers are selected from the group consisting of cellulose ethers.
Preferably, the cellulose ether is selected from one or a combination of hydroxypropyl methyl cellulose ether and methyl cellulose ether.
Still further, the natural polysaccharide comprises one or more of gelatin, carrageenan, locust bean gum, and acacia.
Further, the auxiliary agent is selected from fatty alcohol polyoxyethylene ether, lecithin, laurel sorbitan, palmitotan, stearin sorbitan, polyoxyethylene sorbitan laurate, polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan monostearate and polyoxyethylene-polyoxypropylene copolymer.
Further, the high-concentration essence in the fragrance retention agent accounts for 1-15% by mass percent.
Preferably, the perfume retention agent comprises 1-15% of high-concentration essence, 40-75% of alcohols, 0-20% of ethers, 0-5% of natural polysaccharide and 1-30% of auxiliary agents.
In a fourth aspect, the invention also provides the use of a fragrance retention agent in a fabric.
The invention adopts a method for carrying out essence adsorption and desorption in a thermal environment to prepare the high-power concentrated essence, the adsorption process adopts the zeolite molecular sieve for adsorption, the zeolite molecular sieve is a crystalline aluminosilicate, namely Mx/n [ (AlO 2)x(SiO2)y]·H2 O) is divided into 3A, 4A, 5A and 13x types, the zeolite molecular sieve has a porous structure, uniform pore structure and high size distribution consistency, can have adsorption effect on alcohols, alkenes, benzene organic matters and water, has high hydrothermal stability, has higher adsorption capacity in the gas adsorption process, and has low price compared with other adsorbents such as active carbon, and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. The high-concentration essence is prepared by adopting the adsorption-desorption method of the zeolite molecular sieve (5A), so that the defect of poor fragrance retaining effect of the fragrance retaining agent is greatly improved when the high-concentration essence is used in the fragrance retaining agent, and the problem of the strength of the essence is solved from the source.
2. The invention prepares a liquid fragrance retention agent form without wrapping, can realize fragrance retention effect of more than 50% fragrance in 60 days, and compared with the prior art which needs to adopt microcapsule, microbead and other wrapping modes to realize liquid fragrance retention, the invention has the advantages of simpler technical scheme and low cost, and is suitable for industrial production.
Detailed Description
The experimental methods of the present invention, in which specific conditions are not specified in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The various chemicals commonly used in the examples are commercially available.
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 terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprising" and "having" and any variations thereof, are intended to cover a non-exclusive inclusion. For example, a process, method, apparatus, article, or device that comprises a list of steps is not limited to the elements or modules listed but may alternatively include additional steps not listed or inherent to such process, method, article, or device.
The present invention will be further described in detail with reference to the following embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the description is only illustrative and is not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention.
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
The fragrance retention agent prepared in the embodiment comprises the following components in percentage by mass: 1% of high-concentration essence, 178875% of polyvinyl alcohol, 5% of gelatin and 19% of polyoxyethylene-polyoxypropylene copolymer.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 50% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (5A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 5, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Example 2
The fragrance retention agent prepared in the embodiment comprises the following components in percentage by mass: high-concentration essence 5%, polyvinyl alcohol 1788
55% Of hydroxypropyl methyl cellulose ether 15% of polyoxyethylene sorbitan monopalmitate 25%.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 60% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (5A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 5.5, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Example 3
The fragrance retention agent prepared in the embodiment comprises the following components in percentage by mass: 8% of high-concentration essence and 1788 of polyvinyl alcohol
58 Percent of carrageenan 2 percent, 15 percent of hydroxypropyl methyl cellulose ether and 17 percent of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 80% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (5A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 5.5, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Example 4
The fragrance retention agent prepared in the embodiment comprises the following components in percentage by mass: 10% of high-concentration essence, 50% of polyethylene glycol (molecular weight 800), 5% of gelatin, 15% of hydroxypropyl methyl cellulose ether and 20% of lecithin.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
s1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 100% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (5A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 4.5, stirring for 2.5 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Example 5
The fragrance retention agent prepared in the embodiment comprises the following components in percentage by mass: 10% of high-concentration essence, 40% of polyethylene glycol (molecular weight 2000), 3% of gelatin, 17% of methyl cellulose ether, 28% of fatty alcohol polyoxyethylene ether and 2% of sorbitan palmitat.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 120% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (5A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 6, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Test example one, evaluation of fragrance-retaining Property of fragrance-retaining agent
The fragrance retention agent prepared in the examples 1-5 is subjected to fragrance retention performance test, the fragrance retention agent is diluted by water according to the concentration of 1%, then cotton fabric is added for soaking for 10 minutes, wringing is carried out, the cotton fabric is soaked by clear water twice, the cotton fabric is naturally dried after 10 minutes each time, 10 volunteers with good sense are randomly extracted to evaluate the fragrance concentration of the cotton fabric, the fragrance concentration is scored according to 1-5 minutes, the higher the score is, the better the fragrance retention strength is, and the test result is shown in the following table 1;
Table 1:
the fragrance retention agent prepared in the embodiments 1 to 5 of the present invention is still sufficient in fragrance residue on cotton fabrics after 30 days, and more than 50% of fragrance is still retained on cotton fabrics using the samples of the embodiments 3 to 5 after 60 days, so that the fragrance retention agent of the present invention has good fragrance retention capability in the use process.
Comparative example 1
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence, 1788 58% of polyvinyl alcohol, 2% of carrageenan, 15% of hydroxypropyl methyl cellulose ether and 17% of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 80% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (3A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 5.5, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Comparative example 2
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence, 1788 58% of polyvinyl alcohol, 2% of carrageenan, 15% of hydroxypropyl methyl cellulose ether and 17% of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 80% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (4A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 5.5, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Comparative example 3
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence and 1788 of polyvinyl alcohol
58 Percent of carrageenan 2 percent, 15 percent of hydroxypropyl methyl cellulose ether and 17 percent of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 80% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (13 x) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 5.5, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Test example two, influence of different zeolite molecular sieves on fragrance retaining Property of fragrance retaining agent
The fragrance retention performance of the fragrance retention agents prepared in comparative examples 1-3 and example 3 is compared, different fragrance retention agent samples are diluted with water according to the concentration of 1%, then cotton fabrics are added for soaking for 10 minutes, wringing is carried out, the cotton fabrics are soaked with clear water twice, the cotton fabrics are naturally dried after 10 minutes each time, 10 volunteers with good sense are randomly extracted to evaluate the fragrance concentration of the cotton fabrics, the fragrance concentration is scored according to 1-5 minutes, the higher the score is, the better the fragrance retention strength is, and the test results are shown in the following table 2;
Table 2:
The results of table 2 show that the zeolite molecular sieves (5A) have the best effect, and the fragrance retaining effect is sequentially as follows: zeolite molecular sieve (5A) > zeolite molecular sieve (4A) > zeolite molecular sieve (3A) > zeolite molecular sieve (13 x), the main reasons for this may be that the pore size, uniformity, particle size, and polarity of different types of zeolite molecular sieves are not the same, resulting in different loading effects on the same aroma components.
Comparative example 4
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence and 1788 of polyvinyl alcohol
58 Percent of carrageenan 2 percent, 15 percent of hydroxypropyl methyl cellulose ether and 17 percent of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 80% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
s2, adding a zeolite molecular sieve (5A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 3.5, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Comparative example 5
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence and 1788 of polyvinyl alcohol
58 Percent of carrageenan 2 percent, 15 percent of hydroxypropyl methyl cellulose ether and 17 percent of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 80% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (5A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 7, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Comparative example 6
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence and 1788 of polyvinyl alcohol
58 Percent of carrageenan 2 percent, 15 percent of hydroxypropyl methyl cellulose ether and 17 percent of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent comprises the following steps of:
S1, adding 30% jasmine extractum (jasmine flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain jasmine extractum), rose extractum (rose flower is soaked and extracted by dichloromethane and methanol for 72 hours in sequence, extracting solutions are combined and concentrated to obtain rose extractum) and 80% ethanol (the mass concentration is 75%), heating the reaction kettle to 80 ℃, and stirring for 1 hour at the same time;
S2, adding a zeolite molecular sieve (5A) into the reaction kettle, wherein the zeolite molecular sieve accounts for 15% of the total mass of materials in the reaction kettle, adjusting the pH value to 9, stirring for 3 hours, cooling, and filtering to obtain a liquid;
And S3, adding ethanol solution (the mass fraction is 80%) with the mass of 5 times into a jacketed reaction kettle containing zeolite molecular sieve, continuously heating the reaction kettle to 80 ℃, stirring for 0.5h, filtering, and concentrating the filtrate to obtain the high-power concentrated essence.
Test example III, effect of acid-base on fragrance-retaining Property of fragrance-retaining agent
The fragrance retention performance of the fragrance retention agents prepared in comparative examples 4-6 and example 3 is compared, different fragrance retention agent samples are diluted with water according to the concentration of 1%, then cotton fabrics are added for soaking for 10 minutes, wringing is carried out, the cotton fabrics are soaked with clear water twice, the cotton fabrics are naturally dried after 10 minutes each time, 10 volunteers with good sense are randomly extracted to evaluate the fragrance concentration of the cotton fabrics, the fragrance concentration is scored according to 1-5 minutes, the higher the score is, the better the fragrance retention strength is, and the test result is shown in the following table 3;
Table 3:
The results of table 3 show that when the acidity of the mixture is too high and the alkalinity is too high in the preparation process, the adsorption effect is poor, and the main reason is that the zeolite molecular sieve is an ionic molecular sieve, the polarity of the adsorbate has a great influence on the adsorption effect, and even the polarity of the surface or pore canal of the adsorbate is possibly influenced, so that the adsorption effect on the aroma components is different.
Comparative example 7
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 20% of high-concentration essence, 178824% of polyvinyl alcohol, 1% of carrageenan, 5% of hydroxypropyl methyl cellulose ether and 50% of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent is consistent with example 3.
Comparative example 8
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence, 178874% of polyvinyl alcohol, 3% of carrageenan and 15% of hydroxypropyl methyl cellulose ether.
The preparation method of the high-power essence in the fragrance retention agent is consistent with example 3.
Comparative example 9
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence, 178830% of polyvinyl alcohol, 2% of carrageenan, 43% of hydroxypropyl methyl cellulose ether and 17% of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent is consistent with example 3.
Comparative example 10
The fragrance retention agent prepared in the comparative example comprises the following components in percentage by mass: 8% of high-concentration essence, 178858% of polyvinyl alcohol, 10% of carrageenan, 7% of hydroxypropyl methyl cellulose ether and 17% of fatty alcohol polyoxyethylene ether.
The preparation method of the high-power essence in the fragrance retention agent is consistent with example 3.
Test example IV, influence of the composition of the fragrance-retaining agent on the fragrance-retaining Property
The fragrance retention performance of the fragrance retention agents prepared in comparative examples 7-10 and example 3 is compared, different fragrance retention agent samples are diluted with water according to the concentration of 1%, then cotton fabric is added for soaking for 10 minutes, wringing is carried out, the cotton fabric is soaked with clear water twice, the cotton fabric is naturally dried after 10 minutes each time, 10 volunteers with good sense are randomly extracted to evaluate the fragrance concentration of the cotton fabric, the fragrance concentration is scored according to 1-5 minutes, the higher the score is, the better the fragrance retention strength is, and the test result is shown in the following table 4;
Table 4:
Comparative examples 7 to 10 were tested for the composition and content of the fragrance retention agent prepared according to the present invention to affect the fragrance retention effect of the fragrance retention agent, when the alcohol content in the fragrance retention agent is less than 40% (comparative examples 7 and 9), the high-concentration essence in the fragrance retention agent volatilizes faster, and after 30 days, there is substantially no fragrance residue on the cotton fabric, probably because polyvinyl alcohol and polyethylene glycol are substances with higher molecular weight, have a certain wrapping effect on the fragrance components, and the alcohol substances have a certain binding effect on the polar fragrance volatile components, thus the diffusion performance of fragrance can be exerted for a long time; on the other hand, the auxiliary agent contained in the fragrance-reserving agent component of the present invention is more compatible with the water-soluble and fat-soluble compounds of the fragrance-reserving agent component, so that the fragrance-reserving effect of the fragrance-reserving agent is remarkably reduced without adding the auxiliary agent in comparative example 8. Meanwhile, the comparative example 10 contains a large amount of natural polysaccharide, and the natural polysaccharide component has high adhesive property, and when the component contains more than 5% of natural polysaccharide, the whole system is difficult to uniformly mix, thereby resulting in a decrease in system stability.
It should be noted that, in the present specification, specific features, structures, materials, or characteristics may be arbitrarily combined, and in order to simplify the description, all possible combinations of the features in the foregoing embodiments are not described, and those skilled in the art may combine and combine the features of the different embodiments and the different embodiments described in the present specification without contradiction.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (4)

1. A fragrance retention agent, the fragrance retention agent comprising, in mass fraction: 1-15% of high-concentration essence, 40-75% of alcohols, 15-20% of ethers, 2-5% of natural polysaccharide and 1-30% of auxiliary agents;
The high-concentration essence is prepared from one or more raw materials of jasmine, rosemary, lavender, lily, rose, gardenia, orange peel or concentrated juice;
The alcohols are selected from polyvinyl alcohol, polyethylene glycol 800 or polyethylene glycol 2000;
the ethers are selected from hydroxypropyl methyl cellulose ether or methyl cellulose ether;
The auxiliary agent is selected from fatty alcohol polyoxyethylene ether, lecithin, sorbitan palmitat, polyoxyethylene sorbitan monopalmitate or polyoxyethylene-polyoxypropylene copolymer;
The natural polysaccharide comprises gelatin or carrageenan;
the preparation of the high-concentration essence comprises the following steps:
S1, adding perfume and solvent into a jacketed reaction kettle, heating the reaction kettle to 60-90 ℃, and stirring for 0.5-1 hour;
S2, adding a zeolite molecular sieve 5A into the reaction kettle, wherein the zeolite molecular sieve accounts for 5-20% of the mass of materials in the reaction kettle, adjusting the pH value to be 4.5-6, stirring for 1-5 hours, cooling, filtering, and filtering out liquid;
and S3, adding an ethanol solution into a reaction kettle only containing zeolite molecular sieve, continuously heating the reaction kettle to 60-90 ℃, filtering, and concentrating the filtrate to obtain the high-concentration essence.
2. The fragrance retaining agent of claim 1, comprising, in mass fractions: 8-15% of high-concentration essence, 40-58% of alcohols, 15-20% of ethers, 2-5% of natural polysaccharide and 17-30% of auxiliary agents.
3. The fragrance retaining agent of claim 1, comprising, in mass fractions: 8% of high-concentration essence, 58% of polyvinyl alcohol, 15% of hydroxypropyl methyl cellulose ether, 2% of carrageenan and 17% of fatty alcohol polyoxyethylene ether.
4. Use of a fragrance retaining agent according to claim 1 in a fabric.
CN202310785348.5A 2023-06-29 2023-06-29 Fragrance retaining agent and preparation method and application thereof Active CN116726544B (en)

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