CN118454653A - A grapefruit peel adsorbent and its preparation method and application - Google Patents

A grapefruit peel adsorbent and its preparation method and application Download PDF

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CN118454653A
CN118454653A CN202410698451.0A CN202410698451A CN118454653A CN 118454653 A CN118454653 A CN 118454653A CN 202410698451 A CN202410698451 A CN 202410698451A CN 118454653 A CN118454653 A CN 118454653A
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grapefruit peel
adsorbent
grapefruit
peel adsorbent
adsorption
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张强英
陈莉
崔小梅
布多
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Tibet University
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    • 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
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • 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
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/046Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides

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  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

本发明涉及化学技术领域,具体涉及一种柚子皮吸附剂及其制备方法和应用。所述柚子皮吸附剂的制备方法,包括如下步骤:将柚子皮进行水煮;将水煮后的柚子皮冲洗至中性;把冲洗至中性的柚子皮浸泡于浓度为0.1‑0.5mol/L氯化钙溶液中,然后在温度为65‑75℃、功率为60‑70Hz条件下超声;将超声后的柚子皮再次冲洗至中性后烘干;最后将烘干的柚子皮粉碎后用8‑80目目筛过滤,得柚子皮吸附剂。采用本发明的柚子皮吸附剂对于尼古丁具有很好的吸附性能,可吸附烟尘中的尼古丁,减少其对人体的危害和对环境的污染,具有广阔的应用前景。

The present invention relates to the field of chemical technology, and in particular to a grapefruit peel adsorbent and a preparation method and application thereof. The preparation method of the grapefruit peel adsorbent comprises the following steps: boiling grapefruit peel; rinsing the boiled grapefruit peel to neutrality; soaking the neutralized grapefruit peel in a 0.1-0.5 mol/L calcium chloride solution, and then ultrasonicating at a temperature of 65-75°C and a power of 60-70 Hz; rinsing the ultrasonicated grapefruit peel again to neutrality and drying; finally, crushing the dried grapefruit peel and filtering it with an 8-80 mesh sieve to obtain the grapefruit peel adsorbent. The grapefruit peel adsorbent of the present invention has good adsorption performance for nicotine, can adsorb nicotine in smoke, reduce its harm to the human body and pollution to the environment, and has broad application prospects.

Description

一种柚子皮吸附剂及其制备方法和应用A grapefruit peel adsorbent and its preparation method and application

技术领域Technical Field

本发明涉及化学技术领域,具体涉及一种柚子皮吸附剂及其制备方法和应用。The invention relates to the technical field of chemistry, and in particular to a grapefruit peel adsorbent and a preparation method and application thereof.

背景技术Background Art

尼古丁(Nicotine),也称烟碱,是一种容易上瘾的化学物质。尼古丁气味上辛臭难闻,颜色为无色油状液体,挥发性强,在空气中易转变为棕色,易溶于水及有机溶剂,尼古丁可以使人体的多种器官受到损害,并引发癌症、高血压、慢性支气管炎以及其他肺病等。有研究表明,纯尼古丁只需要几毫克就可以引起头痛、意识涣散等情况,因此吸烟太多的人会发生慢性中毒。尼古丁对人体的危害不仅表现在会让人吸食成瘾,而且还可以造成烟中毒性视神经病变,长期吸烟会引发视力下降,严重的会导致视神经萎缩,最终失明。因此,需要研发出一种能够减少吸烟者对香烟中尼古丁吸入量的产品。Nicotine, also known as nicotine, is an addictive chemical. Nicotine has a pungent smell and is a colorless oily liquid. It is highly volatile and easily turns brown in the air. It is easily soluble in water and organic solvents. Nicotine can damage many organs of the human body and cause cancer, hypertension, chronic bronchitis and other lung diseases. Studies have shown that only a few milligrams of pure nicotine are needed to cause headaches, loss of consciousness, etc., so people who smoke too much will suffer from chronic poisoning. The harm of nicotine to the human body is not only manifested in the addiction of people, but also can cause smoke-induced optic neuropathy. Long-term smoking can cause vision loss, severe cases can cause optic atrophy, and eventually blindness. Therefore, it is necessary to develop a product that can reduce the amount of nicotine inhaled by smokers in cigarettes.

目前,市场上销售的香烟大多数仅仅依靠普通醋酸纤维使其进一步降低烟气中尼古丁,醋酸纤维具有吸味效果较好、外形美观、硬度好等优点,但其生产复杂缓慢、成本高,对香烟中尼古丁的吸附效果较差;活性炭的碳含量高达90%以上,它是一种无毒无味的孔隙物质,吸附效果好,但其制备工艺较复杂、生产成本较高,限制了其大面积使用。At present, most of the cigarettes sold on the market rely solely on ordinary acetate fiber to further reduce nicotine in smoke. Acetate fiber has the advantages of good taste absorption effect, beautiful appearance, good hardness, etc., but its production is complex and slow, the cost is high, and the adsorption effect of nicotine in cigarettes is poor; the carbon content of activated carbon is as high as over 90%. It is a non-toxic and tasteless porous substance with good adsorption effect, but its preparation process is complex and the production cost is high, which limits its large-scale use.

因此,亟需提供一种制备成本低廉且吸附性能好的吸附剂的方法。Therefore, there is an urgent need to provide a method for preparing an adsorbent with low cost and good adsorption performance.

发明内容Summary of the invention

为解决上述问题,本发明的目的在于提供一种柚子皮吸附剂及其制备方法和应用。In order to solve the above problems, the object of the present invention is to provide a grapefruit peel adsorbent and a preparation method and application thereof.

本发明提供了一种柚子皮吸附剂的制备方法,包括如下步骤:The present invention provides a method for preparing a grapefruit peel adsorbent, comprising the following steps:

将柚子皮洗净,除去表面污渍;Wash the grapefruit peel and remove surface stains;

将洗净的柚子皮置于95-100℃水中进行水煮;Boil the washed grapefruit peel in 95-100℃ water;

将水煮后的柚子皮冲洗至中性;Rinse the boiled grapefruit peels until they are neutral;

把冲洗至中性的柚子皮浸泡于浓度为0.1-0.5mol/L氯化钙溶液中,然后放入超声波仪器中超声,所述超声的温度为65-75℃、功率为60-70Hz;The washed grapefruit peel is soaked in a 0.1-0.5 mol/L calcium chloride solution, and then placed in an ultrasonic instrument for ultrasonication, wherein the temperature of the ultrasonication is 65-75° C. and the power is 60-70 Hz;

将超声后的柚子皮再次冲洗至中性;Rinse the grapefruit peels again after ultrasound until they are neutral;

然后再将中性的柚子皮烘干;Then dry the neutral grapefruit peel;

最后将烘干的柚子皮用粉碎机粉碎后用8-80目目筛过滤,得柚子皮吸附剂。Finally, the dried grapefruit peel is crushed by a crusher and filtered through an 8-80 mesh sieve to obtain a grapefruit peel adsorbent.

进一步地,所述氯化钙溶液浓度为0.4mol/L。Furthermore, the concentration of the calcium chloride solution is 0.4 mol/L.

进一步地,所述目筛为40目。Furthermore, the mesh size is 40 mesh.

进一步地,所述超声的温度为68℃、功率为70Hz。Furthermore, the temperature of the ultrasound is 68° C. and the power is 70 Hz.

进一步地,所述超声的时间为20-40min。Furthermore, the ultrasonic treatment time is 20-40 minutes.

进一步地,所述超声的时间为20min。Furthermore, the ultrasonic time is 20 minutes.

进一步地,所述水煮的时间为20-30min。Furthermore, the boiling time is 20-30 minutes.

进一步地,所述水煮的时间为20min。Furthermore, the boiling time is 20 minutes.

本发明还提供了一种柚子皮吸附剂,通过所述制备方法制备得到。The invention also provides a grapefruit peel adsorbent, which is prepared by the preparation method.

本发明还提供了一种所述的柚子皮吸附剂在制备香烟过滤嘴中的应用,所述柚子皮吸附剂用于减少香烟中尼古丁吸入量。The present invention also provides an application of the grapefruit peel adsorbent in preparing a cigarette filter, wherein the grapefruit peel adsorbent is used to reduce the amount of nicotine inhaled in cigarettes.

进一步地,所述柚子皮吸附剂的量为0.05-0.2g。Furthermore, the amount of the grapefruit peel adsorbent is 0.05-0.2g.

进一步地,所述柚子皮吸附剂的量为0.1g。Furthermore, the amount of the grapefruit peel adsorbent is 0.1 g.

进一步地,所述香烟过滤嘴中还含有其它过滤嘴添加剂。Furthermore, the cigarette filter also contains other filter additives.

进一步地,所述其它香烟过滤嘴添加剂选自中草药、矿物类材料、生物试剂、具有吸附性能的过滤材料或纳米材料。Furthermore, the other cigarette filter additives are selected from Chinese herbal medicine, mineral materials, biological reagents, filter materials with adsorption properties or nanomaterials.

与现有技术相比,本发明的有益效果在于:Compared with the prior art, the present invention has the following beneficial effects:

(1)本发明发现采用不同氯化钙浓度处理的柚子皮吸附剂对尼古丁吸附效果有不同的影响,随着氯化钙浓度梯度的上升,对尼古丁的吸附先增加后减少,当氯化钙浓度为0.5mol/L时,吸附率为15.1%,当氯化钙浓度到达0.4mol/L时,吸附率可达34.8%;采用不同吸附剂粒径对尼古丁吸附效果有不同的影响,当柚子皮吸附剂的粒径越来越大时,对尼古丁的吸附总体呈先缓慢上升后缓慢下降的趋势,当粒径为40目时吸附率最大,为40.3%;采用不同柚子皮吸附剂加入量对尼古丁吸附效果有不同的影响,随着柚子皮吸附剂加入量的增加,对尼古丁吸附总体表现为先上升后下降的趋势。当加入量为0.1g、0.15g时,吸附效果较好,而加入量为0.1g时,吸附效果最好,吸附率为39.7%;采用不同吸附剂对尼古丁吸附效果有不同的影响,随着吸附时间的增加,采用本发明的柚子皮吸附剂的吸附率均最高,醋酸纤维对尼古丁的吸附率最低,而同比之下,活性炭没有硅藻土的吸附效果好,而原始柚子皮吸附剂的吸附率大于醋酸纤维的吸附率,小于活性炭和硅藻土的吸附率。(1) The present invention finds that grapefruit peel adsorbent treated with different calcium chloride concentrations has different effects on the nicotine adsorption effect. With the increase of the calcium chloride concentration gradient, the adsorption of nicotine first increases and then decreases. When the calcium chloride concentration is 0.5 mol/L, the adsorption rate is 15.1%. When the calcium chloride concentration reaches 0.4 mol/L, the adsorption rate can reach 34.8%. Different adsorbent particle sizes have different effects on the nicotine adsorption effect. When the particle size of the grapefruit peel adsorbent becomes larger and larger, the adsorption of nicotine generally shows a trend of first slowly increasing and then slowly decreasing. When the particle size is 40 mesh, the adsorption rate is the largest, which is 40.3%. Different grapefruit peel adsorbent addition amounts have different effects on the nicotine adsorption effect. With the increase of the amount of grapefruit peel adsorbent added, the nicotine adsorption generally shows a trend of first increasing and then decreasing. When the addition amount is 0.1g and 0.15g, the adsorption effect is better, and when the addition amount is 0.1g, the adsorption effect is the best, and the adsorption rate is 39.7%; different adsorbents have different effects on the nicotine adsorption effect. With the increase of adsorption time, the adsorption rate of the grapefruit peel adsorbent of the present invention is the highest, and the adsorption rate of nicotine by acetate fiber is the lowest. Compared with the same period, the adsorption effect of activated carbon is not as good as that of diatomaceous earth, and the adsorption rate of the original grapefruit peel adsorbent is greater than that of acetate fiber, but less than that of activated carbon and diatomaceous earth.

(2)本发明的材料制备以农业废弃物柚子皮为原材料,能变废为宝;其次,该材料制备方便,工艺简单,成本低廉,绿色环保且对环境不会造成二次污染。(2) The material preparation of the present invention uses agricultural waste grapefruit peel as raw material, which can turn waste into treasure; secondly, the material preparation is convenient, the process is simple, the cost is low, it is green and environmentally friendly, and it will not cause secondary pollution to the environment.

(3)采用本发明制备的柚子皮吸附剂对于尼古丁具有很好的吸附性能,可吸附烟尘中的尼古丁,减少其对人体的危害,减少其对环境的污染,具有广阔的应用前景。(3) The grapefruit peel adsorbent prepared by the present invention has good adsorption performance for nicotine, can adsorb nicotine in smoke, reduce its harm to the human body, reduce its pollution to the environment, and has broad application prospects.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

图1为本发明吸附装置;FIG1 is an adsorption device of the present invention;

图中,A为橡皮管口;In the figure, A is the opening of the rubber tube;

B为止水夹;B is water-stop clamp;

C为真空泵与止水夹连接处,通过止水夹控制气体流通;C is the connection between the vacuum pump and the water stop clamp, through which the gas flow is controlled;

D为抽滤瓶。D is a suction filtration bottle.

图2为本发明不同氯化钙浓度对烟气中尼古丁吸附效果的影响。FIG. 2 shows the effect of different calcium chloride concentrations on the adsorption of nicotine in smoke according to the present invention.

图3为本发明不同吸附剂粒径对尼古丁吸附率的影响FIG. 3 shows the effect of different adsorbent particle sizes on nicotine adsorption rate of the present invention.

图4为本发明不同柚子皮吸附剂加入量对尼古丁吸附率的影响FIG. 4 shows the effect of different amounts of grapefruit peel adsorbent added on nicotine adsorption rate of the present invention.

图5为本发明不同吸附剂对尼古丁吸附率的影响。FIG. 5 shows the effect of different adsorbents on the nicotine adsorption rate of the present invention.

图6为本发明傅里叶红外光谱分析;FIG6 is a Fourier transform infrared spectrum analysis of the present invention;

图中,1为吸附后柚子皮吸附剂;In the figure, 1 is the grapefruit peel adsorbent after adsorption;

2为柚子皮吸附剂;2 is a grapefruit peel adsorbent;

3线为原始柚子皮吸附剂。Line 3 is the original grapefruit peel adsorbent.

图7为本发明X射线分析;FIG7 is an X-ray analysis of the present invention;

图中,1为吸附后柚子皮吸附剂;In the figure, 1 is the grapefruit peel adsorbent after adsorption;

2为柚子皮吸附剂;2 is a grapefruit peel adsorbent;

3为原始柚子皮吸附剂。3 is the original grapefruit peel adsorbent.

具体实施方式DETAILED DESCRIPTION

为了使本发明的目的及优点更加清楚明白,以下结合实施例对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。如未特殊说明,下述实施例中所用的技术手段为本领域技术人员所熟知的常规手段,下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。In order to make the purpose and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with examples. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. Unless otherwise specified, the technical means used in the following examples are conventional means well known to those skilled in the art, and the materials, reagents, etc. used in the following examples, unless otherwise specified, can all be obtained from commercial sources.

实验材料和仪器:Experimental materials and instruments:

本发明所用的实验材料和仪器如下:The experimental materials and instruments used in the present invention are as follows:

一、实验材料:柚子皮,收集于感恩广场御果汇店铺内柚子皮废弃筐里。1. Experimental materials: pomelo peels, collected from the pomelo peel discarded basket in the Royal Fruit Shop at Thanksgiving Plaza.

二、实验试剂:氢氧化钠,天津瑞金特化学品公司;高锰酸钾,洛阳昊华化学试剂公司;氯化钙,天津瑞金特化学制品公司;活性炭,天津大茂化学试剂厂。2. Experimental reagents: Sodium hydroxide, Tianjin Ruijinte Chemical Company; Potassium permanganate, Luoyang Haohua Chemical Reagent Company; Calcium chloride, Tianjin Ruijinte Chemical Products Company; Activated carbon, Tianjin Damao Chemical Reagent Factory.

三、仪器与设备:电子天平WT3003,杭州市万特横器公司;水浴锅HH-4,上海市实验仪器厂;粉碎机WB1110,上海市精密科学仪器有限公司雷磁仪器厂;干燥箱WPL-65BE,天津泰斯特公司;元素分析仪VarioELcude,德国elementar公司;傅立叶红外光谱仪TENSOR 27,德国布鲁克(Bruker)公司。3. Instruments and equipment: Electronic balance WT3003, Hangzhou Wantehengqi Co., Ltd.; Water bath HH-4, Shanghai Experimental Instrument Factory; Pulverizer WB1110, Shanghai Precision Scientific Instrument Co., Ltd. Leici Instrument Factory; Drying oven WPL-65BE, Tianjin Tester Co., Ltd.; Element analyzer VarioELcude, German elementar company; Fourier transform infrared spectrometer TENSOR 27, German Bruker company.

实施例1:一种柚子皮吸附剂的制备。Example 1: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.1mol/L的氯化钙溶液中,放入68℃、超声波功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.1 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用60目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the grapefruit peel that appears neutral, put it into a constant temperature drying oven for drying, and then crush it with a grinder; finally, filter it with a 60-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

实施例2:一种柚子皮吸附剂的制备。Example 2: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.2mol/L的氯化钙溶液中,放入68℃、超声功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.2 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用60目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the grapefruit peel that appears neutral, put it into a constant temperature drying oven for drying, and then crush it with a grinder; finally, filter it with a 60-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

实施例3:一种柚子皮吸附剂的制备。Example 3: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.3mol/L的氯化钙溶液中,放入68℃、超声功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.3 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用60目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the grapefruit peel that appears neutral, put it into a constant temperature drying oven for drying, and then crush it with a grinder; finally, filter it with a 60-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

实施例4:一种柚子皮吸附剂的制备。Example 4: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.4mol/L的氯化钙溶液中,放入68℃、超声功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.4 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用60目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the grapefruit peel that appears neutral, put it into a constant temperature drying oven for drying, and then crush it with a grinder; finally, filter it with a 60-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

实施例5:一种柚子皮吸附剂的制备。Example 5: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.5mol/L的氯化钙溶液中,放入68℃、超声功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.5 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入55℃恒温干燥箱中烘干至恒重后用粉碎机粉碎;最后用60目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the neutral grapefruit peel, put it into a 55°C constant temperature drying oven and dry it to constant weight, then crush it with a grinder; finally filter it with a 60-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

实施例6:一种柚子皮吸附剂的制备。Example 6: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.4mol/L的氯化钙溶液中,放入68℃、超声功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.4 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用40目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the grapefruit peel that appears neutral, put it into a constant temperature drying oven for drying, and then crush it with a grinder; finally, filter it with a 40-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

实施例7:一种柚子皮吸附剂的制备。Example 7: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.4mol/L的氯化钙溶液中,放入68℃、超声功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.4 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用8目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the grapefruit peel that appears neutral, put it into a constant temperature drying oven for drying, and then crush it with a grinder; finally, filter it with an 8-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

实施例8:一种柚子皮吸附剂的制备。Example 8: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.4mol/L的氯化钙溶液中,放入68℃、超声功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.4 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用18目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the grapefruit peel that appears neutral, put it into a constant temperature drying oven for drying, and then crush it with a grinder; finally, filter it with an 18-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

实施例9:一种柚子皮吸附剂的制备。Example 9: Preparation of a grapefruit peel adsorbent.

1、原料处理:把柚子皮用流动的自来水清洗干净,除去表面污渍;1. Raw material processing: clean the grapefruit peel with running tap water to remove surface stains;

2、水煮:将洗净的柚子皮置于100℃水中20min;2. Boil: Place the washed grapefruit peel in 100℃ water for 20 minutes;

3、冲洗:将水煮后的柚子皮在流动的自来水下冲洗至中性;3. Rinse: Rinse the boiled grapefruit peel under running tap water until it becomes neutral;

4、超声波水解:把已经冲洗至中性的柚子皮浸泡于0.4mol/L的氯化钙溶液中,放入68℃、超声功率为70Hz的超声波仪器中超声20min;4. Ultrasonic hydrolysis: Soak the grapefruit peel that has been washed to neutrality in 0.4 mol/L calcium chloride solution, and put it in an ultrasonic instrument at 68°C and 70 Hz for 20 minutes;

5、冲洗:用流动的自来水清洗超声后的柚子皮至中性;5. Rinse: Use running tap water to wash the grapefruit peel after ultrasound until it becomes neutral;

6、烘干:将显示为中性的柚子皮沥干,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用80目目筛过滤,得改性后的柚子皮渣即柚子皮吸附剂,并保存。6. Drying: drain the grapefruit peel that appears neutral, put it into a constant temperature drying oven for drying, and then crush it with a grinder; finally, filter it with an 80-mesh sieve to obtain the modified grapefruit peel residue, i.e., grapefruit peel adsorbent, and store it.

对比例1:Comparative Example 1:

把柚子皮用流动的自来水清洗干净,除去表面污渍,放入恒温干燥箱中烘干后用粉碎机粉碎;最后用60目目筛过滤,得未改性的柚子皮渣即原始柚子皮吸附剂,并保存。The grapefruit peel is cleaned with running tap water to remove surface stains, placed in a constant temperature drying oven for drying and then crushed with a grinder; finally, filtered with a 60-mesh sieve to obtain unmodified grapefruit peel residue, i.e., original grapefruit peel adsorbent, which is then stored.

对比例2:采用活性炭作为吸附剂;所述活性炭购买自天津大茂化学试剂厂。Comparative Example 2: Activated carbon was used as the adsorbent; the activated carbon was purchased from Tianjin Damao Chemical Reagent Factory.

对比例3:采用醋酸纤维作为吸附剂;所述醋酸纤维为从香烟(红旗渠)中拔出的醋酸纤维。Comparative Example 3: Acetate fiber is used as the adsorbent; the acetate fiber is the acetate fiber pulled out from cigarettes (Hongqi Canal).

对比例4:采用硅藻土作为吸附剂;所述硅藻土购买自赛默飞世尔科技(中国)有限公司。Comparative Example 4: Diatomaceous earth was used as the adsorbent; the diatomaceous earth was purchased from Thermo Fisher Scientific (China) Co., Ltd.

应用例1:吸附率的测定。Application example 1: Determination of adsorption rate.

1、不同氯化钙浓度处理的柚子皮吸附剂对尼古丁吸附效果的影响1. Effect of grapefruit peel adsorbent treated with different calcium chloride concentrations on nicotine adsorption

分别称取0.2g实施例1-实施例5中柚子皮吸附剂,分别放入已经拔出了醋酸纤维的香烟(红旗渠)的过滤口纸套内,之后塞入纸套;Weigh 0.2 g of the grapefruit peel adsorbents in Examples 1 to 5, respectively, and put them into the filter paper sleeves of cigarettes (Hongqiqu) from which the acetate fiber has been removed, and then insert the paper sleeves;

将经拔出醋酸纤维处理后的烟夹在吸附装置(图1)上,并用止水夹夹住,打开真空泵,直至真空泵压力达到0.095MPa后(此时冒出气泡),打开止水夹,点燃香烟,待一支香烟燃尽时就关闭真空泵和止水夹,让烟气完全溶于150mL蒸馏水中,倒入250mL容量瓶中,静置20min;Put the cigarette after the acetate fiber treatment on the adsorption device (Figure 1) and clamp it with a water stop clamp. Turn on the vacuum pump until the vacuum pump pressure reaches 0.095MPa (bubbles appear at this time), open the water stop clamp, light the cigarette, and turn off the vacuum pump and water stop clamp when the cigarette is burned out. Let the smoke completely dissolve in 150mL of distilled water, pour it into a 250mL volumetric flask, and let it stand for 20 minutes.

20min之后加入5g氢氧化钠和0.02765g高锰酸钾,最后定容到250mL刻度线;After 20 minutes, add 5g of sodium hydroxide and 0.02765g of potassium permanganate, and finally adjust the volume to the 250mL mark;

在100℃下水浴8min,冷却到室温后取上层液体进行过滤,取滤液;Place in a water bath at 100°C for 8 minutes, cool to room temperature, filter the upper layer of liquid, and take the filtrate;

采用分光光度法测定香烟烟气中尼古丁的含量。The nicotine content in cigarette smoke was determined by spectrophotometry.

吸附剂对尼古丁的吸附率的计算公式为:吸附率=(M1-M1’)/M1;其中:M1为抽滤装置溶液中尼古丁的总量(1.5+空白),M1’为每次进行实验时抽滤装置溶液中尼古丁的含量。The calculation formula for the adsorption rate of nicotine by the adsorbent is: adsorption rate = (M1-M1')/M1; wherein: M1 is the total amount of nicotine in the filtration device solution (1.5+blank), and M1' is the nicotine content in the filtration device solution during each experiment.

由图2可知,随着氯化钙浓度梯度的上升,对尼古丁的吸附先增加后减少,当氯化钙浓度到达0.4mol/L时,吸附率可达34.8%;当氯化钙浓度为0.5mol/L时,吸附率为15.1%。As shown in Figure 2, with the increase of calcium chloride concentration gradient, the adsorption of nicotine first increases and then decreases. When the calcium chloride concentration reaches 0.4 mol/L, the adsorption rate can reach 34.8%; when the calcium chloride concentration is 0.5 mol/L, the adsorption rate is 15.1%.

2、不同吸附剂粒径对尼古丁吸附效果的影响2. Effect of different adsorbent particle sizes on nicotine adsorption

分别称取0.1g实施例4及实施例6-9中柚子皮吸附剂,分别放入已经拔出了醋酸纤维的香烟(红旗渠)的过滤口纸套内,之后塞入纸套;Weigh 0.1 g of grapefruit peel adsorbents from Examples 4 and 6-9, respectively, and put them into the filter paper sleeves of cigarettes (Hongqiqu) from which acetate fiber has been removed, and then insert the paper sleeves;

将经拔出醋酸纤维处理后的烟夹在吸附装置(图1)上,并用止水夹夹住,打开真空泵,直至真空泵压力达到0.095MPa后(此时冒出气泡),打开止水夹,点燃香烟,待一支香烟燃尽时就关闭真空泵和止水夹,让烟气完全溶于150mL蒸馏水中,倒入250mL容量瓶中,静置20min;Put the cigarette after the acetate fiber treatment on the adsorption device (Figure 1) and clamp it with a water stop clamp. Turn on the vacuum pump until the vacuum pump pressure reaches 0.095MPa (bubbles appear at this time), open the water stop clamp, light the cigarette, and turn off the vacuum pump and water stop clamp when the cigarette is burned out. Let the smoke completely dissolve in 150mL of distilled water, pour it into a 250mL volumetric flask, and let it stand for 20 minutes.

20min之后加入5g氢氧化钠和0.02765g高锰酸钾,最后定容到250mL刻度线;After 20 minutes, add 5g of sodium hydroxide and 0.02765g of potassium permanganate, and finally adjust the volume to the 250mL mark;

在100℃下水浴8min,冷却到室温后取上层液体进行过滤,取滤液;Place in a water bath at 100°C for 8 minutes, cool to room temperature, filter the upper layer of liquid, and take the filtrate;

采用分光光度法测定香烟烟气中尼古丁的含量。The nicotine content in cigarette smoke was determined by spectrophotometry.

由图3可知,当柚子皮吸附剂的粒径越来越大时,对尼古丁的吸附总体呈先缓慢上升后缓慢下降的趋势,且当粒径为40目时吸附率最大,为40.3%。As shown in Figure 3, when the particle size of the grapefruit peel adsorbent becomes larger and larger, the adsorption of nicotine generally shows a trend of first slowly increasing and then slowly decreasing, and the adsorption rate is the largest when the particle size is 40 mesh, which is 40.3%.

3、不同柚子皮吸附剂加入量对尼古丁吸附效果的影响3. Effect of different amounts of grapefruit peel adsorbent on nicotine adsorption

从实施例6中的柚子皮吸附剂分别称取0.05g,0.1g,0.15g,0.2g,0.25g,分别放入已经拔出了醋酸纤维的香烟(红旗渠)的过滤口纸套内,之后塞入纸套;Weigh 0.05g, 0.1g, 0.15g, 0.2g, and 0.25g of the grapefruit peel adsorbent in Example 6, respectively, and put them into the filter paper sleeve of a cigarette (Hongqiqu) from which the acetate fiber has been removed, and then insert the paper sleeve;

将经拔出醋酸纤维处理后的烟夹在吸附装置(图1)上,并用止水夹夹住,打开真空泵,直至真空泵压力达到0.095MPa后(此时冒出气泡),打开止水夹,点燃香烟,待一支香烟燃尽时就关闭真空泵和止水夹,让烟气完全溶于150mL蒸馏水中,倒入250mL容量瓶中,静置20min;Put the cigarette after the acetate fiber treatment on the adsorption device (Figure 1) and clamp it with a water stop clamp. Turn on the vacuum pump until the vacuum pump pressure reaches 0.095MPa (bubbles appear at this time), open the water stop clamp, light the cigarette, and turn off the vacuum pump and water stop clamp when the cigarette is burned out. Let the smoke completely dissolve in 150mL of distilled water, pour it into a 250mL volumetric flask, and let it stand for 20 minutes.

20min之后加入5g氢氧化钠和0.02765g高锰酸钾,最后定容到250mL刻度线;After 20 minutes, add 5g of sodium hydroxide and 0.02765g of potassium permanganate, and finally adjust the volume to the 250mL mark;

在100℃下水浴8min,冷却到室温后取上层液体进行过滤,取滤液;Place in a water bath at 100°C for 8 minutes, cool to room temperature, filter the upper layer of liquid, and take the filtrate;

采用分光光度法测定香烟烟气中尼古丁的含量。The nicotine content in cigarette smoke was determined by spectrophotometry.

由图4可知,随着柚子皮吸附剂加入量的增加,对尼古丁吸附总体表现为先上升后下降的趋势。当加入量为0.1g、0.15g时,吸附效果较好;当加入量为0.1g时,吸附效果最好,吸附率为39.7%。As shown in Figure 4, with the increase in the amount of grapefruit peel adsorbent added, the overall nicotine adsorption shows a trend of first increasing and then decreasing. When the added amount is 0.1g and 0.15g, the adsorption effect is better; when the added amount is 0.1g, the adsorption effect is the best, and the adsorption rate is 39.7%.

4、不同吸附剂对尼古丁吸附效果的影响4. Effect of different adsorbents on nicotine adsorption

分别称取0.1g实施例4中柚子皮吸附剂、对比例1中原始柚子皮吸附剂及对比例2-4中的吸附剂,分别放入已经拔出了醋酸纤维的香烟(所用香烟如表1所示)的过滤口纸套内,之后塞入纸套;将经拔出醋酸纤维处理后的香烟夹在吸附装置上,并用止水夹夹住,打开真空泵,直至真空泵压力达到0.095MPa后(此时冒出气泡),打开止水夹,点燃香烟,待一支香烟燃尽时就关闭真空泵和止水夹,让烟气完全溶于150mL蒸馏水中,倒入250mL容量瓶中,静置20min;0.1 g of the grapefruit peel adsorbent in Example 4, the original grapefruit peel adsorbent in Comparative Example 1, and the adsorbents in Comparative Examples 2-4 were weighed respectively, and were placed in the filter paper sleeves of cigarettes from which acetate fiber had been removed (the cigarettes used were shown in Table 1), and then the paper sleeves were inserted; the cigarettes from which acetate fiber had been removed were clamped on the adsorption device and clamped with a water stop clamp, and the vacuum pump was turned on until the vacuum pump pressure reached 0.095 MPa (bubbles appeared at this time), and the water stop clamp was opened, and the cigarette was lit. When one cigarette was burned out, the vacuum pump and the water stop clamp were turned off, and the smoke was completely dissolved in 150 mL of distilled water, poured into a 250 mL volumetric flask, and allowed to stand for 20 minutes;

20min之后加入5g氢氧化钠和0.02765g高锰酸钾,最后定容到250mL刻度线;After 20 minutes, add 5g of sodium hydroxide and 0.02765g of potassium permanganate, and finally adjust the volume to the 250mL mark;

在100℃下水浴8min,冷却到室温后取上层液体进行过滤,取滤液;Place in a water bath at 100°C for 8 minutes, cool to room temperature, filter the upper layer of liquid, and take the filtrate;

采用分光光度法测定香烟烟气中尼古丁的含量。The nicotine content in cigarette smoke was determined by spectrophotometry.

表1香烟中尼古丁含量Table 1 Nicotine content in cigarettes

香烟品牌Cigarette Brand 产地Origin 尼古丁含量(mg)Nicotine content (mg) 红旗渠Red Flag Canal 河南省中烟工业Henan Tobacco Industry 0.70.7

由图5可知,随着吸附时间的增加,采用本发明的柚子皮吸附剂的吸附率均最高,醋酸纤维对尼古丁的吸附率最低,而同比之下,活性炭没有硅藻土吸附效果好,而原始柚子皮吸附剂的吸附率大于醋酸纤维的吸附率,小于活性炭和硅藻土的吸附率。As shown in Figure 5, with the increase of adsorption time, the adsorption rate of the grapefruit peel adsorbent of the present invention is the highest, and the adsorption rate of nicotine by acetate fiber is the lowest. Compared with the same period, the adsorption effect of activated carbon is not as good as that of diatomaceous earth, and the adsorption rate of the original grapefruit peel adsorbent is greater than that of acetate fiber, but less than that of activated carbon and diatomaceous earth.

应用例2:傅里叶红外光谱分析。Application example 2: Fourier transform infrared spectroscopy analysis.

在研钵中加入200mg溴化钾,分别取2mg处理后的实施例6中柚子皮吸附剂、对比例1中原始柚子皮吸附剂,使其与溴化钾充分研磨,混匀后倒入装片,在压片机上压制成透明状的装片,放在傅立叶红外光谱仪下扫描,测定光谱;200 mg of potassium bromide was added to a mortar, and 2 mg of the treated grapefruit peel adsorbent in Example 6 and the original grapefruit peel adsorbent in Comparative Example 1 were taken respectively, and the mixture was fully ground with potassium bromide, and poured into a tablet, which was pressed into a transparent tablet on a tablet press, and scanned under a Fourier infrared spectrometer to measure the spectrum;

随后再次取应用例1中吸附过尼古丁的柚子皮吸附剂,使其与溴化钾充分研磨,混匀后倒入装片,在压片机上压制成透明状,放在傅立叶红外光谱仪下扫描,测定光谱;Then, the grapefruit peel adsorbent that has absorbed nicotine in Application Example 1 is taken again, and it is fully ground with potassium bromide, poured into tablets after mixing, pressed into a transparent state on a tablet press, and scanned under a Fourier infrared spectrometer to measure the spectrum;

根据放置不同吸附剂的光谱图判断吸附前后以及改性前后的柚子皮吸附剂的性质变化。The changes in the properties of the grapefruit peel adsorbent before and after adsorption and before and after modification were judged based on the spectra of different adsorbents.

由图6的1和2分析可知,吸附波动在1800cm-1~3412cm-1,1500cm-1~1750cm-1,1110cm-1~1400cm-1以及650cm-1~750cm-1处发生变化,即-OH、C=O、C=C、C-H这些基团有峰值的变化,说明这些基团在吸附过程中起到了作用,由此可知化学吸附在此吸附过程中起到重要作用。由图6的2和3对比可知,改性后的柚子皮吸附剂中基团的浓度高于原始柚子皮吸附剂浓度。From the analysis of Figure 6 1 and 2, it can be seen that the adsorption fluctuation changes at 1800cm -1 ~ 3412cm -1 , 1500cm -1 ~ 1750cm -1 , 1110cm -1 ~ 1400cm -1 and 650cm -1 ~ 750cm -1 , that is, the groups -OH, C = O, C = C, CH have peak changes, indicating that these groups play a role in the adsorption process, which shows that chemical adsorption plays an important role in this adsorption process. From the comparison of Figure 6 2 and 3, it can be seen that the concentration of the groups in the modified grapefruit peel adsorbent is higher than that of the original grapefruit peel adsorbent.

应用例3:元素分析。Application example 3: elemental analysis.

称取3mg的对比例1中原始柚子皮吸附剂、实施例6中柚子皮吸附剂、应用例1中吸附过尼古丁的柚子皮吸附剂(吸附后柚子皮吸附剂),放入到锡纸上,包成小正方形作为被测品;将被测品放入元素仪器中分别进行检测,结果如表2。3 mg of the original grapefruit peel adsorbent in Comparative Example 1, the grapefruit peel adsorbent in Example 6, and the grapefruit peel adsorbent adsorbed with nicotine in Application Example 1 (grapefruit peel adsorbent after adsorption) were weighed, placed on tin foil, and wrapped into small squares as the samples to be tested; the samples to be tested were placed in the element instrument for detection, and the results are shown in Table 2.

表2元素含量对比表Table 2 Element content comparison table

N%N% C%C% H%H% S%S% 原始柚子皮吸附剂Original grapefruit peel adsorbent 4.8534.853 34.3134.31 5.4565.456 0.14020.1402 柚子皮吸附剂Grapefruit peel adsorbent 1.8691.869 40.8540.85 6.2026.202 0.06660.0666 吸附后柚子皮吸附剂Grapefruit peel adsorbent after adsorption 2.0322.032 39.139.1 6.0296.029 0.04390.0439

由表2可知,与原始柚子皮吸附剂相比,柚子皮吸附剂、吸附后柚子皮吸附剂的C、H、N、S元素含量均发生了变化,说明改性后的柚子皮吸附剂可能使柚子皮中的C=N、COOH等极性基团数量发生改变,从而对吸附起到了重要作用;柚子皮吸附剂H元素含量增加,说明采用本发明的方法使柚子皮中的羧基、羟基等基团数量增加,而这些基团对吸附尼古丁起到了极大的作用。It can be seen from Table 2 that compared with the original grapefruit peel adsorbent, the contents of C, H, N, and S elements in the grapefruit peel adsorbent and the grapefruit peel adsorbent after adsorption have changed, indicating that the modified grapefruit peel adsorbent may change the number of polar groups such as C=N and COOH in the grapefruit peel, thereby playing an important role in the adsorption; the H element content of the grapefruit peel adsorbent increases, indicating that the method of the present invention increases the number of groups such as carboxyl and hydroxyl in the grapefruit peel, and these groups play a great role in the adsorption of nicotine.

应用例4:X射线分析。Application example 4: X-ray analysis.

按照应用例2中的方法将实施例6中柚子皮吸附剂、对比例1中原始柚子皮吸附剂及应用例1中吸附过尼古丁的柚子皮吸附剂(吸附后柚子皮吸附剂)分别制作成装片,放在X射线衍射仪(XRD)中检测,根据其波峰判断结晶度,从而分析结构性质。According to the method in Application Example 2, the grapefruit peel adsorbent in Example 6, the original grapefruit peel adsorbent in Comparative Example 1, and the grapefruit peel adsorbent after nicotine adsorption in Application Example 1 (grapefruit peel adsorbent after adsorption) were respectively prepared into slides and placed in an X-ray diffractometer (XRD) for detection. The crystallinity was determined based on the peaks, thereby analyzing the structural properties.

由图7分析可知,在2θ=22.5°有较强的特征衍射峰,代表纤维素的结晶区域;原始柚子皮吸附剂的衍射峰值最小,之后是处理后,而吸附后柚子皮吸附剂的衍射峰值最大,柚子皮吸附剂在吸附的整个过程中结晶度增强,物理结构更加稳定,说明了整个吸附过程中柚子皮吸附剂也存在物理吸附。From the analysis of Figure 7, it can be seen that there is a strong characteristic diffraction peak at 2θ=22.5°, representing the crystalline area of cellulose; the diffraction peak of the original grapefruit peel adsorbent is the smallest, followed by the treated one, and the diffraction peak of the grapefruit peel adsorbent after adsorption is the largest. The crystallinity of the grapefruit peel adsorbent is enhanced during the entire adsorption process, and the physical structure is more stable, indicating that physical adsorption also exists in the grapefruit peel adsorbent during the entire adsorption process.

尽管已描述了本发明的优选实施例,但本领域内的技术人员一旦得知了基本创造性概念,则可对这些实施例作出另外的变更和修改。所以,所附权利要求意欲解释为包括优选实施例以及落入本发明范围的所有变更和修改。Although the preferred embodiments of the present invention have been described, those skilled in the art may make other changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the present invention.

显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.

Claims (10)

1.一种柚子皮吸附剂的制备方法,其特征在于,包括如下步骤:1. A method for preparing a grapefruit peel adsorbent, characterized in that it comprises the following steps: 将柚子皮进行水煮;Boil the grapefruit peels; 将水煮后的柚子皮冲洗至中性;Rinse the boiled grapefruit peels until they are neutral; 把冲洗至中性的柚子皮浸泡于浓度为0.1-0.5mol/L氯化钙溶液中,然后在温度为65-75℃、功率为60-70Hz的条件下超声;The washed grapefruit peel is immersed in a 0.1-0.5 mol/L calcium chloride solution, and then ultrasonicated at a temperature of 65-75°C and a power of 60-70 Hz; 将超声后的柚子皮再次冲洗至中性后烘干;The grapefruit peel after ultrasonic treatment is rinsed again until it is neutral and then dried; 最后将烘干的柚子皮粉碎后用8-80目目筛过滤,得柚子皮吸附剂。Finally, the dried grapefruit peel is crushed and filtered through an 8-80 mesh sieve to obtain a grapefruit peel adsorbent. 2.根据权利要求1所述的柚子皮吸附剂的制备方法,其特征在于,所述氯化钙溶液浓度为0.4mol/L。2. The method for preparing a grapefruit peel adsorbent according to claim 1, wherein the concentration of the calcium chloride solution is 0.4 mol/L. 3.根据权利要求1所述的柚子皮吸附剂的制备方法,其特征在于,所述目筛为40目。3. The method for preparing a grapefruit peel adsorbent according to claim 1, wherein the mesh sieve is 40 mesh. 4.根据权利要求1所述的柚子皮吸附剂的制备方法,其特征在于,所述温度为68℃、功率为70Hz。4. The method for preparing a grapefruit peel adsorbent according to claim 1, characterized in that the temperature is 68°C and the power is 70 Hz. 5.根据权利要求1所述的柚子皮吸附剂的制备方法,其特征在于,所述超声的时间为20-40min。5. The method for preparing a grapefruit peel adsorbent according to claim 1, wherein the ultrasonic time is 20-40 min. 6.根据权利要求1所述的柚子皮吸附剂的制备方法,其特征在于,所述水煮的温度为95-100℃、时间为20-30min。6. The method for preparing a grapefruit peel adsorbent according to claim 1, characterized in that the boiling temperature is 95-100°C and the boiling time is 20-30 minutes. 7.一种柚子皮吸附剂,其特征在于,通过权利要求1-6任一项所述制备方法制备得到。7. A grapefruit peel adsorbent, characterized in that it is prepared by the preparation method according to any one of claims 1 to 6. 8.一种权利要求7所述的柚子皮吸附剂在制备香烟过滤嘴中的应用,其特征在于,所述柚子皮吸附剂用于减少香烟中尼古丁吸入量。8. Use of the grapefruit peel adsorbent according to claim 7 in the preparation of cigarette filters, characterized in that the grapefruit peel adsorbent is used to reduce the amount of nicotine inhaled in cigarettes. 9.根据权利要求8所述的柚子皮吸附剂在制备香烟过滤嘴中的应用,其特征在于,所述柚子皮吸附剂的量为0.05-0.2g。9. Use of the grapefruit peel adsorbent in the preparation of cigarette filters according to claim 8, characterized in that the amount of the grapefruit peel adsorbent is 0.05-0.2g. 10.根据权利要求9所述的柚子皮吸附剂在制备香烟过滤嘴中的应用,其特征在于,所述柚子皮吸附剂的量为0.1g。10. Use of the grapefruit peel adsorbent in preparing a cigarette filter according to claim 9, characterized in that the amount of the grapefruit peel adsorbent is 0.1 g.
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