CN112980586A - Purification method of pearl blasting essential oil - Google Patents

Purification method of pearl blasting essential oil Download PDF

Info

Publication number
CN112980586A
CN112980586A CN202110376865.8A CN202110376865A CN112980586A CN 112980586 A CN112980586 A CN 112980586A CN 202110376865 A CN202110376865 A CN 202110376865A CN 112980586 A CN112980586 A CN 112980586A
Authority
CN
China
Prior art keywords
essential oil
zeolite
purified
attapulgite
treatment
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110376865.8A
Other languages
Chinese (zh)
Inventor
苗丽坤
陈�胜
孙炜炜
刘冬
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan Huanghelou Flavoring and Essence Co Ltd
Original Assignee
Wuhan Huanghelou Flavoring and Essence Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan Huanghelou Flavoring and Essence Co Ltd filed Critical Wuhan Huanghelou Flavoring and Essence Co Ltd
Priority to CN202110376865.8A priority Critical patent/CN112980586A/en
Publication of CN112980586A publication Critical patent/CN112980586A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • B01J20/165Natural alumino-silicates, e.g. zeolites

Landscapes

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

Abstract

The invention discloses a purification method of pearl blasting essential oil, which comprises the following steps: performing primary adsorption and filtration treatment on the exploder pearl essential oil in a fluidized bed filter filled with an adsorption material to obtain primary purified essential oil; the adsorption material is a mixed material of modified zeolite and modified attapulgite; performing secondary filtration treatment on the primary purified essential oil through a plate-and-frame filter to obtain secondary purified essential oil; carrying out tertiary filtration treatment on the secondary purified essential oil through ceramic membrane equipment to obtain tertiary purified essential oil; and carrying out vacuum degassing treatment on the purified essential oil obtained in the third step to obtain an essential oil finished product. According to the purification method of the bead blasting essential oil, the bead blasting essential oil is purified through four-step impurity removal treatment, so that easily-oxidizable substances, insoluble impurities and micro bubbles in the bead blasting essential oil are removed, the bead blasting essential oil is uniform and stable in quality, the oil quality of the bead blasting essential oil is improved, the bead blasting dripping forming effect is improved, and the bead blasting forming rate is further improved.

Description

Purification method of pearl blasting essential oil
Technical Field
The invention relates to the technical field of cigarette essence and spice, in particular to a purification method of bead blasting essential oil.
Background
In order to improve the quality and the use effect of the bead blasting essential oil, the olive oil is often used as essential oil base oil. The olive oil contains various vitamins and mineral elements such as calcium, phosphorus, iron, potassium, selenium and the like, and is also rich in various unsaturated, monounsaturated and saturated fatty acids and phospholipids. Wherein, the squalene with the highest oil content has the function of oxidation resistance, but once oxidized, the squalene plays the role of an oxygen-assisting agent. In addition, olive oil contains considerable amount of tocopherol, phytosterol, carotenoid and glycolipid compound, wherein chlorophyll is a photosensitizer and can promote the oxidation of oil under the condition of light. In general, many cyclic olefins exist in olive oil, wherein hydrocarbon olefins containing carbon-carbon double bonds (C = C) are very unstable at normal temperature and pressure, and are easily oxidized with oxygen in the air to form high molecular sticky substances, so that the color of the oil product is gradually deepened.
The quality of the olive oil has certain influence on the process of dropping the exploded beads, and if fine bubbles and precipitated impurities exist in the olive oil, the problems of solid beads, eccentric beads, special-shaped beads and the like can be generated in the dropping process, so that the yield of the exploded beads is influenced. Due to the oxidation of olive oil, the olive oil is gradually viscous and a small amount of precipitate appears, so that the olive oil needs to be purified to remove substances such as oxidation impurities, micro bubbles and other impurities, so as to ensure the uniformity of the bead blasting essential oil and the stability of bead blasting dripping forming. Chinese patent CN201811172101.1 discloses a method for efficiently removing wax in olive oil by using a pulsed electric field and application thereof. The method comprises the steps of carrying out balanced storage on olive oil for 24 hours at the temperature of 20-25 ℃, then adding 0.01-0.05% by weight of a surfactant, and stirring until the surfactant is fully dissolved; then pouring the mixture into a pulsed electric field working chamber, wherein the treatment conditions are as follows: the electric field intensity is 15-30 kV/cm, the treatment temperature is 20-25 ℃, the pulse width is 10-20 mus, the pulse frequency is 300-600 Hz, the circulation treatment is carried out for 1-2 times, and the dewaxed olive oil product is obtained after filtration. The method has the characteristics of simple operation, short time, high efficiency, no introduction of toxic and harmful substances, obvious dewaxing effect, no phenomenon of turbid oil body during storage when the dewaxed olive oil is used as base oil to prepare the bead blasting essential oil, stable forming in the bead blasting forming link of cigarettes, high bead blasting forming rate and capability of effectively ensuring the quality of bead blasting products. This patent is got rid of the waxy component in the olive oil through the pulse electric field effect, carries out purification treatment to the olive oil to improve the oil quality of olive oil, and then improve the shaping rate of exploding the pearl.
However, olive oil contains other oxidative impurities in addition to waxy impurities, and the oxidative impurities cannot be completely removed by the action of a pulsed electric field, so that it is necessary to develop a method for further improving the purity of the popping essential oil after the essential oil is prepared.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a purification method of exploder pearl essential oil.
In order to solve the problems, the invention adopts the following technical scheme:
a purification method of popping essential oil comprises the following steps:
performing primary adsorption and filtration treatment on the exploder pearl essential oil in a fluidized bed filter filled with an adsorption material to obtain primary purified essential oil; the adsorption material is a mixed material of modified zeolite and modified attapulgite;
performing secondary filtration treatment on the primary purified essential oil through a plate-and-frame filter to obtain secondary purified essential oil;
carrying out tertiary filtration treatment on the secondary purified essential oil through ceramic membrane equipment to obtain tertiary purified essential oil;
and carrying out vacuum degassing treatment on the three purified essential oils to obtain an essential oil finished product.
Preferably, the mass ratio of the modified zeolite to the modified attapulgite is 1: 1-3: 1.
Preferably, the modified zeolite is prepared by the following method:
drying natural zeolite, crushing the dried natural zeolite to 250-300 meshes, and roasting the natural zeolite at 350-450 ℃ for 1.5-2 h to obtain roasted zeolite;
placing the roasted zeolite in a quaternary ammonium salt cationic surfactant solution, uniformly stirring, and placing in a constant-temperature oscillator for oscillation treatment for 8-10 h;
and taking out the zeolite subjected to the oscillation treatment, standing for more than 12 hours, washing with water until the pH value is 6-7, and drying at 60-70 ℃ for more than 12 hours.
Preferably, the mass ratio of the calcined zeolite to the quaternary ammonium salt cationic surfactant is 1:12 to 1: 15.
Preferably, the quaternary ammonium salt type cationic surfactant is cetylpyridinium bromide.
Preferably, the modified attapulgite is prepared by the following method:
crushing attapulgite to 300-350 meshes, and placing the crushed attapulgite in dilute sulfuric acid with the concentration of 0.8-1.3 mol/L for acidification treatment for 3-5 hours;
and (3) washing the acidified attapulgite until the pH value is 6-7, roasting at 250-260 ℃ for 2-3 h, cooling, and storing in a dryer.
Preferably, the solid-to-liquid ratio of the attapulgite to the dilute sulfuric acid is 1: 10-1: 15.
Preferably, the filtration precision of the plate-and-frame filter is 100 um.
Preferably, the ceramic membrane element of the ceramic membrane device has a pore size of 100 nm.
Preferably, the time of the vacuum degassing treatment is 30-40 min.
Compared with the prior art, the invention has the technical effects that:
the purification method of the exploded bead essential oil comprises the steps of firstly, carrying out primary adsorption and filtration impurity removal treatment on the exploded bead essential oil through an adsorption material, and removing substances such as free fatty acid, wax and the like in the exploded bead essential oil through the adsorption material; then removing fine particle insoluble impurities in the bead blasting essential oil through a plate frame filter and a ceramic membrane device in sequence, and further purifying the bead blasting essential oil; finally, removing micro-bubble impurities in the bead blasting essential oil through vacuum degassing. According to the purification method of the bead blasting essential oil, the bead blasting essential oil is purified through four-step impurity removal treatment, so that easily-oxidizable substances, insoluble impurities and micro bubbles in the bead blasting essential oil are removed, the bead blasting essential oil is uniform and stable in quality, the oil quality of the bead blasting essential oil is improved, the bead blasting dripping forming effect is improved, and the bead blasting forming rate is further improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
It will be appreciated by those skilled in the art that the objects and advantages that can be achieved with the present invention are not limited to the specific details set forth above, and that these and other objects that can be achieved with the present invention will be more clearly understood from the detailed description that follows.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a purification method of popping essential oil, which comprises the following steps:
(1) performing primary adsorption and filtration treatment on the exploder pearl essential oil in a fluidized bed filter filled with an adsorption material to obtain primary purified essential oil; the adsorption material is a mixed material of modified zeolite and modified attapulgite; preferably, the mass ratio of the modified zeolite to the modified attapulgite is 1: 1-3: 1.
(2) Performing secondary filtration treatment on the primary purified essential oil through a plate-and-frame filter to obtain secondary purified essential oil; preferably, the filtering precision of the plate-and-frame filter adopted in the embodiment of the invention is 100 um;
(3) carrying out tertiary filtration treatment on the secondary purified essential oil through ceramic membrane equipment to obtain tertiary purified essential oil; preferably, the aperture of the ceramic membrane element of the ceramic membrane equipment adopted in the embodiment of the invention is 100 nm;
(4) and carrying out vacuum degassing treatment on the purified essential oil obtained in the third step to obtain an essential oil finished product. Preferably, the time of the vacuum degassing treatment is 30-40 min.
The bead blasting essential oil used by the invention is obtained by taking olive oil as base oil and adding and uniformly mixing Dendranthema indicum essence according to 2% of the mass of the base oil.
The modified zeolite used in the invention is prepared by the following method:
(10) drying natural zeolite, crushing the dried natural zeolite into 250-300 meshes, roasting the natural zeolite at 350-450 ℃ for 1.5-2 hours to obtain roasted zeolite, and enabling the zeolite to become loose and porous sponge bodies through roasting treatment so as to improve the cation exchange and adsorption capacity of the zeolite;
(11) placing the roasted zeolite in a quaternary ammonium salt cationic surfactant solution, uniformly stirring, and placing in a constant-temperature oscillator for oscillation treatment for 8-10 h; in a preferred embodiment of the invention, the quaternary ammonium salt cationic surfactant is cetylpyridinium bromide, and the mass ratio of the calcined zeolite to the quaternary ammonium salt cationic surfactant is 1: 12-1: 15; soaking the calcined and activated zeolite by using a quaternary ammonium salt cationic surfactant, and loading the quaternary ammonium salt cationic surfactant on the surface of the calcined zeolite in an ion exchange mode to remove water molecules, inorganic and organic impurities on the surface and in the calcined zeolite, so that the pore channel of the calcined zeolite is unobstructed, the porosity is improved, the surface activity is enhanced, the selective adsorption capacity of the calcined zeolite is improved, the ion exchange rate is accelerated, the ion exchange performance is improved, and the adsorption capacity of the calcined zeolite on hydrophobic organic matters is improved;
(12) and taking out the zeolite subjected to oscillation treatment, standing for more than 12h, washing with water until the pH value is 6-7, and drying at 60-70 ℃ for more than 12h to obtain the cation-loaded modified zeolite.
The modified attapulgite used in the invention is prepared by the following method:
(20) crushing attapulgite to 300-350 meshes, and placing the crushed attapulgite in dilute sulfuric acid with the concentration of 0.8-1.3 mol/L for acidification treatment for 3-5 hours; preferably, the solid-to-liquid ratio of the attapulgite to the dilute sulfuric acid is 1: 10-1: 15.
(21) Washing the acidified attapulgite with water until the pH value is 6-7, roasting at 250-260 ℃ for 2-3 h, cooling, and storing in a dryer.
Natural attapulgite belongs to hydrous magnesium aluminum silicate fibrous clay minerals, and has special mineral morphology and crystal structure, most of the states are that only four of five octahedral positions are occupied, and the vacancy positions are in trans positions. The special crystal structure and the stacking mode form a large number of pore channel structures, the needle-rod-shaped and fibrous crystal particles form the interstitial holes in the aggregate, and the pore diameter range covers micropores, mesopores and macropores.
The modified attapulgite obtained by extrusion crushing, acid treatment, water washing neutralization and medium-temperature roasting of the material bed enables symbiotic cement in the minerals to be dissolved out, and continuous crystal beams of the attapulgite are dispersed into a fluffy single crystal structure due to the action of acid etching. Meanwhile, the hair-shaped crystal substances converted from the montmorillonite to the attapulgite by the acid treatment are hydrolyzed to form more recrystallized attapulgite crystals, namely more fine microneedle rod-shaped and fibrous crystals, and the specific surface area is further improved. The acid reaction not only increases the pore size and the nanopore structure, but also causes the change of the property of the surface functional group, and the octahedral cation H+For positive ion Mg2+,Al3+,Fe3+Displacement from edge to center in sequence until completely substituted, and H+Not completely occupying the octahedral sites of the cations, but rather more of the O anions co-ordinating with the original-The combination forms silanol alkyl Si-OH, and the Si-OH functional group can well adsorb organic matters. In addition, R-OH structures generated by hydrolysis of Si-O broken bonds and Al-O, Mg-O broken bonds also form a large amount of L-acid-base active centers and B-acid-base active centers, and in the adsorption and catalysis in the grease decoloring process, the active sites are the positions where the adsorption and catalysis of the attapulgite occur, and are one of the important conditions that the modified attapulgite has excellent adsorption performance. The attapulgite is acidized by dilute sulfuric acid, and then is activated at a medium temperature of 250-260 ℃, so that fiber bundles of the attapulgite are depolymerized, the pore volume of the attapulgite is improved, the surface area of the attapulgite is increased, pores and broken bonds of the attapulgite are more exposed, and the adsorbability and the ion exchange capacity of the attapulgite are improved.
The natural zeolite has SiO as basic structure4Silicon-oxygen tetrahedron and AlO4Aluminum tetrahedronThe three-dimensional porous structure is characterized in that the three-dimensional porous structure and the three-dimensional porous structure are connected through oxygen bridges to form a cavity with a three-dimensional net structure, the cavities are communicated with each other through various micro pore channels to form a criss-cross spatial network microporous structure, and the micropores are uniform in size, large in specific surface area and high in adsorption performance. The negative charge center on the anion lattice of the zeolite is not overlapped with the positive charge center of the balancing cation in space, so that the zeolite has larger electrostatic attraction, simultaneously has large dispersion force, has selective adsorption effect on polar, unsaturated and easily polarized molecules and has poorer adsorption performance on hydrophobic organic matters. The adsorption capacity of the modified zeolite to hydrophobic organic matters is greatly improved by modifying the surface of the zeolite and introducing nonpolar hydrophobic groups. Zeolites are capable of strong interactions with unsaturated compounds, i.e., molecules of organic compounds that can be polarized, containing double bonds, triple bonds, etc.
The invention has the obvious advantages that the modified zeolite and the modified attapulgite are compounded to be used as a primary adsorption and filtration material, and the purification treatment of the bead blasting essential oil can be realized at room temperature. In the existing technology, when bentonite, clay and other adsorbents are used for carrying out decolorization and degumming treatment, the oil needs to be heated to 80-110 ℃ so as to better meet the adsorption generated in the decolorization process of the oil and the energy exchange condition accompanied by the action in the reaction process. The transmittance of the olive oil can be obviously increased (the transmittance at the wavelength of 500nm is improved by 47.9 percent, and the transmittance at the wavelength of 400nm is improved by 70.3 percent) by the purification method.
The invention adopts the mixed adsorption material of modified zeolite and modified attapulgite to carry out multi-point adsorption, competitive adsorption and ion exchange adsorption on easily oxidizable substances such as free fatty acid, phospholipid, carotenoid, chlorophyll, tocopherol, cycloolefins and the like in the bead blasting essential oil so as to remove the easily oxidizable substances in the bead blasting essential oil in advance and prevent the easily oxidizable substances from being gradually oxidized in the bead blasting essential oil to generate insoluble impurities.
The purification method of the exploded bead essential oil comprises the steps of firstly, carrying out primary adsorption and filtration impurity removal treatment on the exploded bead essential oil through an adsorption material, and removing substances such as free fatty acid, wax and the like in the exploded bead essential oil through the adsorption material; then removing fine particle insoluble impurities in the bead blasting essential oil through a plate frame filter and a ceramic membrane device in sequence, and further purifying the bead blasting essential oil; finally, removing micro-bubble impurities in the bead blasting essential oil through vacuum degassing. According to the purification method of the bead blasting essential oil, the bead blasting essential oil is purified through four-step impurity removal treatment, so that easily-oxidizable substances, insoluble impurities and micro bubbles in the bead blasting essential oil are removed, the bead blasting essential oil is uniform and stable in quality, the oil quality of the bead blasting essential oil is improved, the bead blasting dripping forming effect is improved, and the bead blasting forming rate is further improved.
The following is a further description with reference to specific examples.
Example 1
The embodiment 1 of the invention provides a purification method of popping essential oil, which comprises the following steps:
(1) performing primary adsorption and filtration treatment on the exploder pearl essential oil in a fluidized bed filter filled with an adsorption material to obtain primary purified essential oil; the adsorption material is a mixed material of modified zeolite and modified attapulgite, and the mass ratio of the modified zeolite to the modified attapulgite is 1: 1;
(2) performing secondary filtration treatment on the primary purified essential oil through a plate-and-frame filter with the filtration precision of 100um to obtain secondary purified essential oil;
(3) carrying out tertiary filtration treatment on the secondary purified essential oil through ceramic membrane equipment with a ceramic membrane element aperture of 100nm to obtain tertiary purified essential oil;
(4) and carrying out vacuum degassing treatment on the three purified essential oils for 30min to obtain the finished essential oil.
Wherein, the modified zeolite in the step (1) is prepared by adopting the following method:
(10) drying natural zeolite, crushing the dried natural zeolite to 250-300 meshes, and roasting the natural zeolite at 350 ℃ for 2 hours to obtain roasted zeolite;
(11) placing the roasted zeolite in a cetylpyridinium bromide solution, uniformly stirring, and placing in a constant-temperature (25 ℃) oscillator for oscillation treatment for 8 hours; the mass ratio of the calcined zeolite to the cetylpyridinium bromide is 1: 12;
(12) and taking out the zeolite subjected to oscillation treatment, standing at room temperature for 12h, washing with water until the pH value is 6-7, and drying at 60 ℃ for 12h to obtain the cation-loaded modified zeolite.
The modified attapulgite in the step (1) is prepared by the following method:
(20) crushing attapulgite to 300-350 meshes, and placing the crushed attapulgite in dilute sulfuric acid with the concentration of 0.8mol/L for acidification treatment for 5 hours; the solid-to-liquid ratio of the attapulgite to the dilute sulfuric acid is 1: 10.
(21) Washing the acidified attapulgite with water until the pH value is 6-7, roasting at 250 ℃ for 3h, cooling, and storing in a dryer.
Example 2
The embodiment 2 of the invention provides a purification method of popping essential oil, which comprises the following steps:
(1) performing primary adsorption and filtration treatment on the exploder pearl essential oil in a fluidized bed filter filled with an adsorption material to obtain primary purified essential oil; the adsorption material is a mixed material of modified zeolite and modified attapulgite, and the mass ratio of the modified zeolite to the modified attapulgite is 2: 1;
(2) performing secondary filtration treatment on the primary purified essential oil through a plate-and-frame filter with the filtration precision of 100um to obtain secondary purified essential oil;
(3) carrying out tertiary filtration treatment on the secondary purified essential oil through ceramic membrane equipment with a ceramic membrane element aperture of 100nm to obtain tertiary purified essential oil;
(4) and carrying out vacuum degassing treatment on the three purified essential oils for 35min to obtain the finished essential oil.
Wherein, the modified zeolite in the step (1) is prepared by adopting the following method:
(10) drying natural zeolite, crushing the dried natural zeolite into 250-300 meshes, and roasting the natural zeolite at 400 ℃ for 2 hours to obtain roasted zeolite;
(11) placing the roasted zeolite in a cetylpyridinium bromide solution, uniformly stirring, and placing in a constant-temperature (25 ℃) oscillator for oscillation treatment for 9 hours; the mass ratio of the calcined zeolite to the cetylpyridinium bromide is 1: 13;
(12) and taking out the zeolite subjected to oscillation treatment, standing at room temperature for 18h, washing with water until the pH value is 6-7, and drying at 60 ℃ for 24h to obtain the cation-loaded modified zeolite.
The modified attapulgite in the step (1) is prepared by the following method:
(20) crushing attapulgite to 300-350 meshes, and placing the crushed attapulgite in dilute sulfuric acid with the concentration of 1.1mol/L for acidification treatment for 4 hours; the solid-to-liquid ratio of the attapulgite to the dilute sulfuric acid is 1: 12.
(21) Washing the acidified attapulgite with water until the pH value is 6-7, roasting at 260 ℃ for 2h, cooling, and storing in a dryer.
Example 3
The embodiment 3 of the invention provides a purification method of popping essential oil, which comprises the following steps:
(1) performing primary adsorption and filtration treatment on the exploder pearl essential oil in a fluidized bed filter filled with an adsorption material to obtain primary purified essential oil; the adsorption material is a mixed material of modified zeolite and modified attapulgite, and the mass ratio of the modified zeolite to the modified attapulgite is 3: 1;
(2) performing secondary filtration treatment on the primary purified essential oil through a plate-and-frame filter with the filtration precision of 100um to obtain secondary purified essential oil;
(3) carrying out tertiary filtration treatment on the secondary purified essential oil through ceramic membrane equipment with a ceramic membrane element aperture of 100nm to obtain tertiary purified essential oil;
(4) and carrying out vacuum degassing treatment on the three purified essential oils for 40min to obtain the finished essential oil.
Wherein, the modified zeolite in the step (1) is prepared by adopting the following method:
(10) drying natural zeolite, crushing the dried natural zeolite to 250-300 meshes, and roasting the natural zeolite at 450 ℃ for 1.5 hours to obtain roasted zeolite;
(11) placing the roasted zeolite in a cetylpyridinium bromide solution, uniformly stirring, and placing in a constant-temperature (25 ℃) oscillator for oscillation treatment for 10 hours; the mass ratio of the calcined zeolite to the cetylpyridinium bromide is 1: 15;
(12) and taking out the zeolite subjected to oscillation treatment, standing at room temperature for 18h, washing with water until the pH value is 6-7, and drying at 70 ℃ for 12h to obtain the cation-loaded modified zeolite.
The modified attapulgite in the step (1) is prepared by the following method:
(20) crushing attapulgite to 300-350 meshes, and placing the crushed attapulgite in dilute sulfuric acid with the concentration of 1.3mol/L for acidification treatment for 3 hours; the solid-to-liquid ratio of the attapulgite to the dilute sulfuric acid is 1: 15.
(21) Washing the acidified attapulgite with water until the pH value is 6-7, roasting at 260 ℃ for 3h, cooling, and storing in a dryer.
The purified finished exploded bead essential oil products obtained in embodiments 1 to 3 of the present invention are sequentially labeled as A, B, C, and with reference to a conventional production process of cigarette exploded beads in an enterprise, together with a raw solution of the exploded bead essential oil (labeled as D) without being purified, the finished product of the exploded bead essential oil is prepared into the exploded bead A, B, C, D for cigarettes according to a preparation process of dropping pills, wherein the raw solution of the cigarette exploded bead essential oil is prepared from a dropping pill wrapping material placed in a dropping pill machine mucilage jar and a curing agent placed in a pill container, and the indexes such as average pressure, moisture, rubber specific gravity, molding rate and the like of the four exploded beads A, B, C, D are detected, and the detection results are shown in table 1.
Figure DEST_PATH_IMAGE002
The detection result shows that the finished product of the bead blasting essential oil subjected to purification treatment has good adaptability to bead blasting wall materials and forming equipment. As seen from the table 1, the popping beads prepared from the popping bead essential oil purified by the method are more stable in on-line forming, higher in popping bead forming rate, free of phenomena of solid beads, large notches or core deviation and the like, excellent in various indexes of the finished popping beads, more round in appearance and more than 98% in the whole popping bead forming rate.
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.

Claims (10)

1. The purification method of the pearl blasting essential oil is characterized by comprising the following steps:
performing primary adsorption and filtration treatment on the exploder pearl essential oil in a fluidized bed filter filled with an adsorption material to obtain primary purified essential oil; the adsorption material is a mixed material of modified zeolite and modified attapulgite;
performing secondary filtration treatment on the primary purified essential oil through a plate-and-frame filter to obtain secondary purified essential oil;
carrying out tertiary filtration treatment on the secondary purified essential oil through ceramic membrane equipment to obtain tertiary purified essential oil;
and carrying out vacuum degassing treatment on the three purified essential oils to obtain an essential oil finished product.
2. The method for purifying popping bead essential oil according to claim 1, wherein the mass ratio of the modified zeolite to the modified attapulgite is 1: 1-3: 1.
3. The method for purifying exploder bead essential oil disclosed by claim 2, wherein the modified zeolite is prepared by the following method:
drying natural zeolite, crushing the dried natural zeolite to 250-300 meshes, and roasting the natural zeolite at 350-450 ℃ for 1.5-2 h to obtain roasted zeolite;
placing the roasted zeolite in a quaternary ammonium salt cationic surfactant solution, uniformly stirring, and placing in a constant-temperature oscillator for oscillation treatment for 8-10 h;
and taking out the zeolite subjected to the oscillation treatment, standing for more than 12 hours, washing with water until the pH value is 6-7, and drying at 60-70 ℃ for more than 12 hours.
4. The method for purifying exploder bead essential oil according to claim 3, wherein the mass ratio of the roasted zeolite to the quaternary ammonium salt cationic surfactant is 1: 12-1: 15.
5. The method for purifying exploder bead essential oil disclosed by claim 4, wherein the quaternary ammonium salt type cationic surfactant is cetylpyridinium bromide.
6. The method for purifying blasting bead essential oil according to claim 2, wherein the modified attapulgite is prepared by the following method:
crushing attapulgite to 300-350 meshes, and placing the crushed attapulgite in dilute sulfuric acid with the concentration of 0.8-1.3 mol/L for acidification treatment for 3-5 hours;
and (3) washing the acidified attapulgite until the pH value is 6-7, roasting at 250-260 ℃ for 2-3 h, cooling, and storing in a dryer.
7. The method for purifying blasting bead essential oil according to claim 6, wherein the solid-to-liquid ratio of the attapulgite to the dilute sulfuric acid is 1: 10-1: 15.
8. The method for purifying popping essential oil, which is characterized in that the filtration precision of the plate-and-frame filter is 100um according to claim 1.
9. The method for purifying popping essential oil, which is claimed in claim 1, wherein the pore size of the ceramic membrane element of the ceramic membrane device is 100 nm.
10. The method for purifying popping essential oil, which is characterized in that the vacuum degassing treatment time is 30-40 min.
CN202110376865.8A 2021-04-08 2021-04-08 Purification method of pearl blasting essential oil Pending CN112980586A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110376865.8A CN112980586A (en) 2021-04-08 2021-04-08 Purification method of pearl blasting essential oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110376865.8A CN112980586A (en) 2021-04-08 2021-04-08 Purification method of pearl blasting essential oil

Publications (1)

Publication Number Publication Date
CN112980586A true CN112980586A (en) 2021-06-18

Family

ID=76339474

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110376865.8A Pending CN112980586A (en) 2021-04-08 2021-04-08 Purification method of pearl blasting essential oil

Country Status (1)

Country Link
CN (1) CN112980586A (en)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049111A (en) * 1990-07-03 1991-02-13 四川建筑材料工业学院 The acid soak acid heat activation of Concave-convex clay rod
CN104804871A (en) * 2015-04-27 2015-07-29 湖北中烟工业有限责任公司 Spicy spice for kretek blasting bead, preparation method and application thereof
CN106590927A (en) * 2017-01-08 2017-04-26 山东乐悠悠花生油科技有限公司 Fine finishing method for high-quality peanut oil
CN107510091A (en) * 2017-08-16 2017-12-26 湖北中烟工业有限责任公司 A kind of preparation method of the quick-fried pearl essential oil of cigarette
CN108101072A (en) * 2018-01-22 2018-06-01 太原理工大学 The preparation method of micro--meso-hole structure analcime
CN108179066A (en) * 2018-01-16 2018-06-19 武汉黄鹤楼香精香料有限公司 It is a kind of for honeysuckle Peppermint essential oil of the quick-fried pearl of cigarette and its preparation method and application
CN109111990A (en) * 2018-10-09 2019-01-01 湖北中烟工业有限责任公司 Utilize the method and its application of wax in impulse electric field efficient removal olive oil
CN110105414A (en) * 2011-12-19 2019-08-09 可口可乐公司 Purify the method and its purposes of sweetleaf steviol glycoside
CN112280621A (en) * 2020-11-19 2021-01-29 禹州战营迷迭香生物科技有限公司 Rosemary essential oil extraction process

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049111A (en) * 1990-07-03 1991-02-13 四川建筑材料工业学院 The acid soak acid heat activation of Concave-convex clay rod
CN110105414A (en) * 2011-12-19 2019-08-09 可口可乐公司 Purify the method and its purposes of sweetleaf steviol glycoside
CN104804871A (en) * 2015-04-27 2015-07-29 湖北中烟工业有限责任公司 Spicy spice for kretek blasting bead, preparation method and application thereof
CN106590927A (en) * 2017-01-08 2017-04-26 山东乐悠悠花生油科技有限公司 Fine finishing method for high-quality peanut oil
CN107510091A (en) * 2017-08-16 2017-12-26 湖北中烟工业有限责任公司 A kind of preparation method of the quick-fried pearl essential oil of cigarette
CN108179066A (en) * 2018-01-16 2018-06-19 武汉黄鹤楼香精香料有限公司 It is a kind of for honeysuckle Peppermint essential oil of the quick-fried pearl of cigarette and its preparation method and application
CN108101072A (en) * 2018-01-22 2018-06-01 太原理工大学 The preparation method of micro--meso-hole structure analcime
CN109111990A (en) * 2018-10-09 2019-01-01 湖北中烟工业有限责任公司 Utilize the method and its application of wax in impulse electric field efficient removal olive oil
CN112280621A (en) * 2020-11-19 2021-01-29 禹州战营迷迭香生物科技有限公司 Rosemary essential oil extraction process

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
方巧, 等: "溴化十六烷基吡啶改性沸石对水中甲基橙的吸附", 环境工程学报, vol. 08, no. 06, pages 1 *

Similar Documents

Publication Publication Date Title
JP4404991B2 (en) Active white clay shaped particles, production method thereof and use thereof
CN104028250B (en) For removing filter medium, filter core and the preparation method of Aluminium in Drinking Water
JPS63291641A (en) Synthetic adsorbent of metal-oxide-silica
KR20090030131A (en) Method for preparing surface-modified transparent bead type aerogel and aerogel prepared therefrom
CN105770957B (en) A kind of air cleaning compound and its preparation method and application
KR101201246B1 (en) Interspersed clays
EP0378633B1 (en) Zeolite granules with zeolite binder
CN112980586A (en) Purification method of pearl blasting essential oil
CN104667635B (en) For removing the filter medium of organochlorine, filter element and preparation method in drinking water
EP2906341B1 (en) Binder-free compact zeolite preforms and method for the production thereof
CN104083944B (en) For removing the filter medium of Pb in Drinking Water, filter core and preparation method
JP3540040B2 (en) Adsorbent manufacturing method
DE102016202516A1 (en) Hierarchized ZSM-58 zeolite
CN104587959A (en) Filter medium for removing endosulfan from water as well as filter element and preparation method of filter medium
CN102727519A (en) External diatomite medicament and preparation method thereof
CN106278213A (en) Red wine decanting device
KR100969638B1 (en) Heterogeneous adsorbent and the use thereof for diffusion separation methods
RU2203224C1 (en) Method of preparing high-phase purity granulated faujasite
US20030133868A1 (en) Mesostructured metal or non-metal oxides and method for making same
JPS6246489B2 (en)
CN104530471A (en) Method for decolorizing dyed gelatin soft capsule shell wastes
JP3657033B2 (en) Production method of clay intercalated porous body
KR960010078B1 (en) Process for the preparation of x-type zeolite absorbent
RU2203220C1 (en) Method of preparing granulated high-phase purity a and x-structure zeolite adsorbent
JP2697040B2 (en) Ion exchange method for zeolite compacts

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20210618

RJ01 Rejection of invention patent application after publication